Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805011128/lh6402sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805011128/lh6402Isup2.hkl |
CCDC reference: 272021
Data collection: SMART (Bruker, 1999); 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: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: UdMX (local program).
[Ni(C16H22N6)2][NiCl4]·CH4O·H2O | F(000) = 1899 |
Mr = 906.07 | Dx = 1.447 Mg m−3 |
Monoclinic, P21/c | Cu Kα radiation, λ = 1.54178 Å |
Hall symbol: -P 2ybc | Cell parameters from 36297 reflections |
a = 10.2998 (2) Å | θ = 2.4–72.6° |
b = 18.5245 (3) Å | µ = 3.85 mm−1 |
c = 21.9660 (3) Å | T = 220 K |
β = 94.118 (1)° | Plate, blue |
V = 4180.26 (12) Å3 | 0.30 × 0.30 × 0.08 mm |
Z = 4 |
Bruker SMART 2K/Platform CCD area-detector diffractometer | 8242 independent reflections |
Radiation source: sealed tube | 7048 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.091 |
Detector resolution: 5.5 pixels mm-1 | θmax = 72.6°, θmin = 3.1° |
ω scans | h = −12→12 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −22→21 |
Tmin = 0.287, Tmax = 0.740 | l = −27→26 |
49482 measured reflections |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.051 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.156 | H-atom parameters constrained |
S = 1.13 | w = 1/[σ2(Fo2) + (0.1017P)2 + 0.294P] where P = (Fo2 + 2Fc2)/3 |
8242 reflections | (Δ/σ)max = 0.001 |
485 parameters | Δρmax = 1.05 e Å−3 |
2 restraints | Δρmin = −0.57 e Å−3 |
Experimental. X-ray crystallographic data for I were collected from a single-crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 2 K Charged-Coupled Device (CCD) Area Detector using the program SMART and normal focus sealed tube source graphite monochromated Cu—Kα radiation. The crystal-to-detector distance was 4.908 cm, and the data collection was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning. The initial unit-cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 9.0 degree scan in 30 frames over four different parts of the reciprocal space (120 frames total). One complete sphere of data was collected, to better than 0.8 Å resolution. Upon completion of the data collection, the first 101 frames were recollected in order to improve the decay correction analysis. The structure contains 34 electrons displaced on four different sites of 53 Å3 , which were attributed to four disordered water molecules per unit cell. The PLATON/Squeeze (Spek, 2003) operation has been carried out to model these molecules and solve the disorder issue. |
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. Hydrogen bond details: H97D.·Cl2 2.505 O97.·Cl2 3.332 (3) O97—H97D.·Cl2 173.9 |
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 | 1.0000 | 0.5000 | 0.5000 | 0.02969 (10) | |
N1 | 0.84141 (15) | 0.44415 (9) | 0.45692 (7) | 0.0361 (4) | |
N2 | 0.75964 (14) | 0.41052 (8) | 0.49442 (7) | 0.0320 (3) | |
N3 | 0.97738 (14) | 0.59002 (9) | 0.44310 (7) | 0.0365 (4) | |
N4 | 1.08906 (14) | 0.61892 (8) | 0.42337 (7) | 0.0317 (3) | |
N5 | 1.13211 (15) | 0.46284 (8) | 0.43795 (7) | 0.0364 (4) | |
N6 | 1.21832 (14) | 0.51278 (8) | 0.41874 (7) | 0.0311 (3) | |
C1 | 0.8539 (3) | 0.45594 (17) | 0.34510 (10) | 0.0682 (8) | |
H1A | 0.9355 | 0.4799 | 0.3572 | 0.102* | |
H1B | 0.7962 | 0.4895 | 0.3227 | 0.102* | |
H1C | 0.8704 | 0.4149 | 0.3193 | 0.102* | |
C2 | 0.7919 (2) | 0.43049 (12) | 0.40067 (9) | 0.0441 (5) | |
C3 | 0.6785 (2) | 0.38900 (12) | 0.40213 (9) | 0.0455 (5) | |
H3 | 0.6253 | 0.3728 | 0.3683 | 0.055* | |
C4 | 0.66017 (17) | 0.37659 (11) | 0.46202 (9) | 0.0375 (4) | |
C5 | 0.5570 (2) | 0.33501 (14) | 0.49058 (11) | 0.0559 (6) | |
H5A | 0.5971 | 0.2994 | 0.5184 | 0.084* | |
H5B | 0.5024 | 0.3108 | 0.4591 | 0.084* | |
H5C | 0.5043 | 0.3677 | 0.5130 | 0.084* | |
C6 | 1.0915 (3) | 0.33253 (12) | 0.42014 (14) | 0.0629 (7) | |
H6A | 1.0200 | 0.3417 | 0.4455 | 0.094* | |
H6B | 1.1495 | 0.2969 | 0.4397 | 0.094* | |
H6C | 1.0576 | 0.3145 | 0.3807 | 0.094* | |
C7 | 1.1650 (2) | 0.40132 (11) | 0.41166 (10) | 0.0424 (5) | |
C8 | 1.2721 (2) | 0.41145 (11) | 0.37708 (9) | 0.0418 (5) | |
H8 | 1.3136 | 0.3761 | 0.3547 | 0.050* | |
C9 | 1.30475 (18) | 0.48283 (11) | 0.38218 (8) | 0.0358 (4) | |
C10 | 1.4092 (2) | 0.52464 (13) | 0.35493 (11) | 0.0525 (6) | |
H10A | 1.3712 | 0.5657 | 0.3328 | 0.079* | |
H10B | 1.4531 | 0.4940 | 0.3271 | 0.079* | |
H10C | 1.4713 | 0.5415 | 0.3871 | 0.079* | |
C11 | 0.7432 (2) | 0.61966 (16) | 0.43184 (14) | 0.0678 (8) | |
H11A | 0.7298 | 0.5685 | 0.4383 | 0.102* | |
H11B | 0.6878 | 0.6356 | 0.3968 | 0.102* | |
H11C | 0.7214 | 0.6463 | 0.4678 | 0.102* | |
C12 | 0.8825 (2) | 0.63294 (12) | 0.42041 (10) | 0.0444 (5) | |
C13 | 0.9332 (2) | 0.68830 (12) | 0.38660 (10) | 0.0490 (5) | |
H13 | 0.8857 | 0.7253 | 0.3659 | 0.059* | |
C14 | 1.0652 (2) | 0.67893 (10) | 0.38914 (8) | 0.0385 (4) | |
C15 | 1.1701 (3) | 0.71997 (12) | 0.36165 (12) | 0.0564 (6) | |
H15A | 1.2313 | 0.7379 | 0.3938 | 0.085* | |
H15B | 1.1324 | 0.7603 | 0.3384 | 0.085* | |
H15C | 1.2151 | 0.6885 | 0.3348 | 0.085* | |
C16 | 1.21270 (16) | 0.58590 (9) | 0.44066 (8) | 0.0293 (4) | |
H16 | 1.2806 | 0.6139 | 0.4214 | 0.035* | |
Ni2 | 1.0000 | 0.5000 | 0.0000 | 0.03056 (10) | |
N21 | 0.99622 (14) | 0.45153 (9) | 0.08592 (7) | 0.0349 (3) | |
N22 | 1.11431 (14) | 0.43399 (8) | 0.11478 (7) | 0.0327 (3) | |
N23 | 1.15014 (15) | 0.56432 (8) | 0.04077 (7) | 0.0355 (4) | |
N24 | 1.24117 (14) | 0.53040 (8) | 0.07845 (7) | 0.0326 (3) | |
N25 | 0.85380 (15) | 0.57610 (9) | 0.01538 (7) | 0.0359 (4) | |
N26 | 0.75850 (14) | 0.58431 (8) | −0.03054 (7) | 0.0339 (3) | |
C21 | 0.7660 (2) | 0.43614 (15) | 0.10752 (12) | 0.0551 (6) | |
H21A | 0.7371 | 0.4821 | 0.1229 | 0.083* | |
H21B | 0.7200 | 0.3972 | 0.1263 | 0.083* | |
H21C | 0.7480 | 0.4344 | 0.0636 | 0.083* | |
C22 | 0.90868 (18) | 0.42801 (11) | 0.12266 (9) | 0.0378 (4) | |
C23 | 0.9693 (2) | 0.39611 (12) | 0.17472 (9) | 0.0416 (5) | |
H23 | 0.9281 | 0.3759 | 0.2075 | 0.050* | |
C24 | 1.1004 (2) | 0.39999 (11) | 0.16884 (8) | 0.0384 (4) | |
C25 | 1.2136 (2) | 0.37426 (15) | 0.20925 (11) | 0.0615 (7) | |
H25A | 1.2688 | 0.3440 | 0.1860 | 0.092* | |
H25B | 1.1825 | 0.3466 | 0.2428 | 0.092* | |
H25C | 1.2632 | 0.4154 | 0.2253 | 0.092* | |
C26 | 1.1081 (2) | 0.69081 (12) | 0.00798 (12) | 0.0537 (6) | |
H26A | 1.0920 | 0.6758 | −0.0342 | 0.081* | |
H26B | 1.1566 | 0.7357 | 0.0096 | 0.081* | |
H26C | 1.0257 | 0.6978 | 0.0260 | 0.081* | |
C27 | 1.1847 (2) | 0.63414 (11) | 0.04262 (9) | 0.0394 (4) | |
C28 | 1.2973 (2) | 0.64331 (11) | 0.08114 (10) | 0.0433 (5) | |
H28 | 1.3407 | 0.6871 | 0.0901 | 0.052* | |
C29 | 1.33216 (18) | 0.57706 (11) | 0.10331 (9) | 0.0379 (4) | |
C30 | 1.4421 (2) | 0.55469 (13) | 0.14730 (12) | 0.0541 (6) | |
H30A | 1.4081 | 0.5285 | 0.1810 | 0.081* | |
H30B | 1.4885 | 0.5972 | 0.1628 | 0.081* | |
H30C | 1.5011 | 0.5238 | 0.1267 | 0.081* | |
C31 | 0.8930 (3) | 0.62224 (14) | 0.12066 (10) | 0.0580 (6) | |
H31A | 0.9708 | 0.5928 | 0.1198 | 0.087* | |
H31B | 0.8414 | 0.6057 | 0.1532 | 0.087* | |
H31C | 0.9176 | 0.6722 | 0.1278 | 0.087* | |
C32 | 0.8154 (2) | 0.61600 (11) | 0.06126 (9) | 0.0414 (5) | |
C33 | 0.6957 (2) | 0.64820 (13) | 0.04463 (10) | 0.0482 (5) | |
H33 | 0.6481 | 0.6785 | 0.0691 | 0.058* | |
C34 | 0.66092 (19) | 0.62771 (11) | −0.01338 (10) | 0.0437 (5) | |
C35 | 0.5422 (2) | 0.64314 (17) | −0.05376 (14) | 0.0706 (8) | |
H35A | 0.5633 | 0.6769 | −0.0853 | 0.106* | |
H35B | 0.4760 | 0.6639 | −0.0298 | 0.106* | |
H35C | 0.5098 | 0.5986 | −0.0725 | 0.106* | |
C36 | 0.76798 (17) | 0.54663 (10) | −0.08759 (8) | 0.0317 (4) | |
H36 | 0.6935 | 0.5616 | −0.1158 | 0.038* | |
Ni3 | 0.42641 (4) | 0.77631 (2) | 0.245018 (15) | 0.04356 (9) | |
Cl1 | 0.49993 (7) | 0.71671 (4) | 0.33024 (3) | 0.07339 (19) | |
Cl2 | 0.21731 (6) | 0.75424 (4) | 0.20784 (3) | 0.06300 (17) | |
Cl3 | 0.55720 (6) | 0.75212 (3) | 0.16896 (3) | 0.05183 (14) | |
Cl4 | 0.43912 (6) | 0.89555 (3) | 0.26514 (3) | 0.05340 (14) | |
C97 | 0.0810 (3) | 0.56757 (17) | 0.25579 (12) | 0.0685 (8) | |
H97A | 0.1145 | 0.5600 | 0.2977 | 0.103* | |
H97B | 0.0296 | 0.5261 | 0.2419 | 0.103* | |
H97C | 0.0268 | 0.6105 | 0.2534 | 0.103* | |
O97 | 0.1815 (3) | 0.57619 (15) | 0.22006 (15) | 0.1196 (10) | |
H97D | 0.1956 | 0.6199 | 0.2155 | 0.179* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.03121 (19) | 0.0318 (2) | 0.0265 (2) | −0.00488 (15) | 0.00538 (16) | 0.00149 (15) |
N1 | 0.0388 (7) | 0.0447 (8) | 0.0256 (7) | −0.0136 (6) | 0.0069 (6) | 0.0010 (6) |
N2 | 0.0344 (7) | 0.0372 (7) | 0.0251 (7) | −0.0080 (6) | 0.0070 (6) | −0.0009 (6) |
N3 | 0.0317 (7) | 0.0405 (8) | 0.0378 (8) | −0.0006 (6) | 0.0058 (6) | 0.0084 (6) |
N4 | 0.0364 (7) | 0.0305 (7) | 0.0290 (7) | −0.0016 (6) | 0.0079 (6) | 0.0030 (6) |
N5 | 0.0422 (7) | 0.0313 (7) | 0.0368 (8) | −0.0063 (6) | 0.0109 (6) | −0.0030 (6) |
N6 | 0.0366 (7) | 0.0302 (7) | 0.0278 (7) | −0.0019 (6) | 0.0095 (6) | −0.0004 (6) |
C1 | 0.0777 (15) | 0.099 (2) | 0.0281 (10) | −0.0350 (15) | 0.0081 (11) | 0.0000 (12) |
C2 | 0.0499 (10) | 0.0562 (12) | 0.0265 (9) | −0.0123 (9) | 0.0041 (8) | −0.0030 (8) |
C3 | 0.0441 (10) | 0.0595 (12) | 0.0325 (10) | −0.0139 (9) | 0.0007 (8) | −0.0108 (9) |
C4 | 0.0340 (8) | 0.0424 (10) | 0.0364 (9) | −0.0066 (7) | 0.0050 (7) | −0.0083 (8) |
C5 | 0.0475 (10) | 0.0738 (15) | 0.0472 (12) | −0.0265 (10) | 0.0097 (9) | −0.0085 (11) |
C6 | 0.0824 (16) | 0.0306 (10) | 0.0781 (17) | −0.0112 (11) | 0.0229 (14) | −0.0087 (10) |
C7 | 0.0533 (11) | 0.0316 (9) | 0.0431 (11) | −0.0019 (8) | 0.0083 (9) | −0.0043 (8) |
C8 | 0.0520 (10) | 0.0378 (9) | 0.0363 (10) | 0.0078 (8) | 0.0092 (8) | −0.0058 (8) |
C9 | 0.0382 (8) | 0.0405 (9) | 0.0293 (9) | 0.0049 (8) | 0.0073 (7) | −0.0010 (7) |
C10 | 0.0524 (11) | 0.0543 (12) | 0.0544 (13) | −0.0021 (10) | 0.0291 (10) | −0.0053 (10) |
C11 | 0.0374 (10) | 0.0856 (18) | 0.0807 (18) | 0.0135 (11) | 0.0060 (11) | 0.0276 (15) |
C12 | 0.0400 (9) | 0.0502 (11) | 0.0428 (11) | 0.0057 (9) | 0.0020 (8) | 0.0088 (9) |
C13 | 0.0561 (11) | 0.0483 (11) | 0.0431 (11) | 0.0165 (9) | 0.0067 (9) | 0.0123 (9) |
C14 | 0.0561 (11) | 0.0314 (8) | 0.0290 (8) | 0.0030 (8) | 0.0112 (8) | 0.0040 (7) |
C15 | 0.0771 (14) | 0.0420 (11) | 0.0536 (13) | 0.0046 (11) | 0.0294 (11) | 0.0168 (9) |
C16 | 0.0332 (8) | 0.0306 (8) | 0.0249 (8) | −0.0046 (6) | 0.0080 (6) | −0.0005 (6) |
Ni2 | 0.03101 (19) | 0.0343 (2) | 0.0262 (2) | 0.00491 (16) | 0.00076 (17) | −0.00090 (15) |
N21 | 0.0304 (7) | 0.0428 (8) | 0.0313 (8) | 0.0027 (6) | 0.0007 (6) | 0.0017 (6) |
N22 | 0.0340 (7) | 0.0368 (8) | 0.0270 (7) | −0.0005 (6) | −0.0012 (6) | −0.0002 (6) |
N23 | 0.0379 (7) | 0.0346 (8) | 0.0334 (8) | 0.0026 (6) | −0.0020 (6) | 0.0006 (6) |
N24 | 0.0329 (7) | 0.0315 (7) | 0.0329 (7) | 0.0014 (6) | −0.0004 (6) | 0.0000 (6) |
N25 | 0.0388 (7) | 0.0399 (8) | 0.0287 (7) | 0.0083 (6) | 0.0004 (6) | −0.0029 (6) |
N26 | 0.0309 (7) | 0.0360 (8) | 0.0347 (8) | 0.0051 (6) | 0.0021 (6) | −0.0019 (6) |
C21 | 0.0372 (10) | 0.0735 (15) | 0.0560 (13) | −0.0015 (10) | 0.0138 (9) | 0.0031 (12) |
C22 | 0.0376 (9) | 0.0418 (10) | 0.0348 (9) | −0.0009 (8) | 0.0080 (7) | −0.0041 (8) |
C23 | 0.0506 (10) | 0.0486 (11) | 0.0264 (9) | −0.0091 (9) | 0.0079 (8) | −0.0028 (7) |
C24 | 0.0480 (10) | 0.0417 (10) | 0.0252 (8) | −0.0054 (8) | 0.0010 (7) | −0.0002 (7) |
C25 | 0.0630 (13) | 0.0804 (17) | 0.0389 (11) | −0.0104 (12) | −0.0114 (10) | 0.0195 (11) |
C26 | 0.0668 (13) | 0.0377 (10) | 0.0555 (13) | 0.0040 (10) | −0.0030 (11) | 0.0034 (10) |
C27 | 0.0481 (10) | 0.0350 (9) | 0.0356 (10) | 0.0007 (8) | 0.0050 (8) | −0.0006 (7) |
C28 | 0.0523 (10) | 0.0375 (9) | 0.0399 (10) | −0.0092 (8) | 0.0025 (9) | −0.0027 (8) |
C29 | 0.0380 (9) | 0.0401 (10) | 0.0353 (9) | −0.0047 (8) | 0.0008 (8) | −0.0025 (8) |
C30 | 0.0494 (11) | 0.0505 (12) | 0.0594 (14) | −0.0091 (10) | −0.0160 (10) | 0.0014 (10) |
C31 | 0.0783 (15) | 0.0649 (14) | 0.0299 (10) | 0.0197 (12) | −0.0027 (10) | −0.0112 (10) |
C32 | 0.0531 (11) | 0.0404 (10) | 0.0314 (9) | 0.0091 (8) | 0.0077 (8) | −0.0040 (8) |
C33 | 0.0507 (11) | 0.0507 (11) | 0.0443 (11) | 0.0120 (9) | 0.0112 (9) | −0.0094 (9) |
C34 | 0.0367 (9) | 0.0437 (10) | 0.0511 (12) | 0.0099 (8) | 0.0067 (8) | −0.0067 (9) |
C35 | 0.0481 (11) | 0.0858 (18) | 0.0758 (17) | 0.0327 (12) | −0.0094 (12) | −0.0213 (14) |
C36 | 0.0316 (7) | 0.0340 (8) | 0.0290 (8) | 0.0019 (7) | −0.0002 (6) | 0.0008 (7) |
Ni3 | 0.0580 (2) | 0.04482 (19) | 0.02817 (17) | −0.00942 (16) | 0.00548 (15) | 0.00153 (13) |
Cl1 | 0.0811 (4) | 0.0822 (4) | 0.0555 (3) | −0.0005 (3) | −0.0041 (3) | 0.0297 (3) |
Cl2 | 0.0620 (3) | 0.0824 (4) | 0.0447 (3) | −0.0229 (3) | 0.0042 (3) | 0.0039 (3) |
Cl3 | 0.0698 (3) | 0.0452 (3) | 0.0426 (3) | −0.0082 (2) | 0.0183 (2) | −0.00509 (19) |
Cl4 | 0.0662 (3) | 0.0486 (3) | 0.0452 (3) | −0.0028 (2) | 0.0031 (2) | −0.0095 (2) |
C97 | 0.0834 (17) | 0.0806 (18) | 0.0416 (13) | −0.0146 (14) | 0.0045 (13) | −0.0075 (12) |
O97 | 0.1276 (19) | 0.0930 (17) | 0.147 (2) | 0.0082 (15) | 0.0738 (18) | 0.0250 (17) |
Ni1—N3 | 2.0870 (16) | Ni2—N25ii | 2.1077 (15) |
Ni1—N3i | 2.0870 (16) | N21—C22 | 1.326 (2) |
Ni1—N1i | 2.1004 (15) | N21—N22 | 1.370 (2) |
Ni1—N1 | 2.1004 (15) | N22—C24 | 1.361 (2) |
Ni1—N5i | 2.1094 (16) | N22—C36ii | 1.435 (2) |
Ni1—N5 | 2.1094 (16) | N23—C27 | 1.341 (3) |
N1—C2 | 1.327 (2) | N23—N24 | 1.359 (2) |
N1—N2 | 1.369 (2) | N24—C29 | 1.360 (2) |
N2—C4 | 1.359 (2) | N24—C36ii | 1.445 (2) |
N2—C16i | 1.436 (2) | N25—C32 | 1.332 (2) |
N3—C12 | 1.328 (2) | N25—N26 | 1.365 (2) |
N3—N4 | 1.367 (2) | N26—C34 | 1.361 (2) |
N4—C14 | 1.355 (2) | N26—C36 | 1.444 (2) |
N4—C16 | 1.439 (2) | C21—C22 | 1.491 (3) |
N5—C7 | 1.332 (2) | C21—H21A | 0.9700 |
N5—N6 | 1.370 (2) | C21—H21B | 0.9700 |
N6—C9 | 1.359 (2) | C21—H21C | 0.9700 |
N6—C16 | 1.440 (2) | C22—C23 | 1.395 (3) |
C1—C2 | 1.494 (3) | C23—C24 | 1.368 (3) |
C1—H1A | 0.9700 | C23—H23 | 0.9400 |
C1—H1B | 0.9700 | C24—C25 | 1.492 (3) |
C1—H1C | 0.9700 | C25—H25A | 0.9700 |
C2—C3 | 1.400 (3) | C25—H25B | 0.9700 |
C3—C4 | 1.362 (3) | C25—H25C | 0.9700 |
C3—H3 | 0.9400 | C26—C27 | 1.489 (3) |
C4—C5 | 1.487 (3) | C26—H26A | 0.9700 |
C5—H5A | 0.9700 | C26—H26B | 0.9700 |
C5—H5B | 0.9700 | C26—H26C | 0.9700 |
C5—H5C | 0.9700 | C27—C28 | 1.396 (3) |
C6—C7 | 1.501 (3) | C28—C29 | 1.359 (3) |
C6—H6A | 0.9700 | C28—H28 | 0.9400 |
C6—H6B | 0.9700 | C29—C30 | 1.494 (3) |
C6—H6C | 0.9700 | C30—H30A | 0.9700 |
C7—C8 | 1.397 (3) | C30—H30B | 0.9700 |
C8—C9 | 1.367 (3) | C30—H30C | 0.9700 |
C8—H8 | 0.9400 | C31—C32 | 1.485 (3) |
C9—C10 | 1.486 (3) | C31—H31A | 0.9700 |
C10—H10A | 0.9700 | C31—H31B | 0.9700 |
C10—H10B | 0.9700 | C31—H31C | 0.9700 |
C10—H10C | 0.9700 | C32—C33 | 1.394 (3) |
C11—C12 | 1.496 (3) | C33—C34 | 1.353 (3) |
C11—H11A | 0.9700 | C33—H33 | 0.9400 |
C11—H11B | 0.9700 | C34—C35 | 1.486 (3) |
C11—H11C | 0.9700 | C35—H35A | 0.9700 |
C12—C13 | 1.390 (3) | C35—H35B | 0.9700 |
C13—C14 | 1.368 (3) | C35—H35C | 0.9700 |
C13—H13 | 0.9400 | C36—N22ii | 1.435 (2) |
C14—C15 | 1.484 (3) | C36—N24ii | 1.445 (2) |
C15—H15A | 0.9700 | C36—H36 | 0.9900 |
C15—H15B | 0.9700 | Ni3—Cl4 | 2.2547 (7) |
C15—H15C | 0.9700 | Ni3—Cl1 | 2.2568 (7) |
C16—N2i | 1.436 (2) | Ni3—Cl3 | 2.2649 (7) |
C16—H16 | 0.9900 | Ni3—Cl2 | 2.2847 (7) |
Ni2—N21 | 2.0929 (16) | C97—O97 | 1.353 (4) |
Ni2—N21ii | 2.0929 (16) | C97—H97A | 0.9700 |
Ni2—N23ii | 2.1010 (15) | C97—H97B | 0.9700 |
Ni2—N23 | 2.1010 (15) | C97—H97C | 0.9700 |
Ni2—N25 | 2.1076 (15) | O97—H97D | 0.8300 |
N3—Ni1—N3i | 180 | N21ii—Ni2—N25 | 85.26 (6) |
N3—Ni1—N1i | 85.76 (6) | N23ii—Ni2—N25 | 86.28 (6) |
N3i—Ni1—N1i | 94.24 (6) | N23—Ni2—N25 | 93.72 (6) |
N3—Ni1—N1 | 94.24 (6) | N21—Ni2—N25ii | 85.26 (6) |
N3i—Ni1—N1 | 85.76 (6) | N21ii—Ni2—N25ii | 94.74 (6) |
N1i—Ni1—N1 | 180 | N23ii—Ni2—N25ii | 93.71 (6) |
N3—Ni1—N5i | 94.40 (6) | N23—Ni2—N25ii | 86.28 (6) |
N3i—Ni1—N5i | 85.60 (6) | N25—Ni2—N25ii | 180 |
N1i—Ni1—N5i | 93.73 (6) | C22—N21—N22 | 105.09 (15) |
N1—Ni1—N5i | 86.27 (6) | C22—N21—Ni2 | 138.35 (13) |
N3—Ni1—N5 | 85.59 (6) | N22—N21—Ni2 | 116.47 (11) |
N3i—Ni1—N5 | 94.40 (6) | C24—N22—N21 | 111.62 (15) |
N1i—Ni1—N5 | 86.27 (6) | C24—N22—C36ii | 128.59 (15) |
N1—Ni1—N5 | 93.73 (6) | N21—N22—C36ii | 119.78 (14) |
N5i—Ni1—N5 | 180 | C27—N23—N24 | 104.91 (15) |
C2—N1—N2 | 105.14 (15) | C27—N23—Ni2 | 138.19 (13) |
C2—N1—Ni1 | 138.43 (13) | N24—N23—Ni2 | 116.86 (11) |
N2—N1—Ni1 | 116.43 (11) | N23—N24—C29 | 112.08 (15) |
C4—N2—N1 | 111.63 (15) | N23—N24—C36ii | 119.48 (14) |
C4—N2—C16i | 129.05 (15) | C29—N24—C36ii | 128.44 (15) |
N1—N2—C16i | 119.32 (14) | C32—N25—N26 | 105.11 (15) |
C12—N3—N4 | 105.03 (15) | C32—N25—Ni2 | 138.29 (13) |
C12—N3—Ni1 | 138.63 (14) | N26—N25—Ni2 | 116.12 (11) |
N4—N3—Ni1 | 116.26 (11) | C34—N26—N25 | 111.55 (16) |
C14—N4—N3 | 111.97 (15) | C34—N26—C36 | 128.55 (16) |
C14—N4—C16 | 128.10 (16) | N25—N26—C36 | 119.86 (14) |
N3—N4—C16 | 119.91 (14) | C22—C21—H21A | 109.5 |
C7—N5—N6 | 104.70 (15) | C22—C21—H21B | 109.5 |
C7—N5—Ni1 | 139.02 (14) | H21A—C21—H21B | 109.5 |
N6—N5—Ni1 | 116.18 (11) | C22—C21—H21C | 109.5 |
C9—N6—N5 | 111.89 (15) | H21A—C21—H21C | 109.5 |
C9—N6—C16 | 128.69 (15) | H21B—C21—H21C | 109.5 |
N5—N6—C16 | 119.33 (14) | N21—C22—C23 | 110.74 (17) |
C2—C1—H1A | 109.5 | N21—C22—C21 | 122.25 (18) |
C2—C1—H1B | 109.5 | C23—C22—C21 | 127.01 (19) |
H1A—C1—H1B | 109.5 | C24—C23—C22 | 106.71 (17) |
C2—C1—H1C | 109.5 | C24—C23—H23 | 126.6 |
H1A—C1—H1C | 109.5 | C22—C23—H23 | 126.6 |
H1B—C1—H1C | 109.5 | N22—C24—C23 | 105.85 (17) |
N1—C2—C3 | 110.43 (18) | N22—C24—C25 | 122.73 (19) |
N1—C2—C1 | 122.81 (19) | C23—C24—C25 | 131.42 (19) |
C3—C2—C1 | 126.75 (19) | C24—C25—H25A | 109.5 |
C4—C3—C2 | 106.76 (17) | C24—C25—H25B | 109.5 |
C4—C3—H3 | 126.6 | H25A—C25—H25B | 109.5 |
C2—C3—H3 | 126.6 | C24—C25—H25C | 109.5 |
N2—C4—C3 | 106.04 (16) | H25A—C25—H25C | 109.5 |
N2—C4—C5 | 123.59 (18) | H25B—C25—H25C | 109.5 |
C3—C4—C5 | 130.37 (18) | C27—C26—H26A | 109.5 |
C4—C5—H5A | 109.5 | C27—C26—H26B | 109.5 |
C4—C5—H5B | 109.5 | H26A—C26—H26B | 109.5 |
H5A—C5—H5B | 109.5 | C27—C26—H26C | 109.5 |
C4—C5—H5C | 109.5 | H26A—C26—H26C | 109.5 |
H5A—C5—H5C | 109.5 | H26B—C26—H26C | 109.5 |
H5B—C5—H5C | 109.5 | N23—C27—C28 | 110.04 (17) |
C7—C6—H6A | 109.5 | N23—C27—C26 | 122.31 (18) |
C7—C6—H6B | 109.5 | C28—C27—C26 | 127.64 (19) |
H6A—C6—H6B | 109.5 | C29—C28—C27 | 107.10 (18) |
C7—C6—H6C | 109.5 | C29—C28—H28 | 126.4 |
H6A—C6—H6C | 109.5 | C27—C28—H28 | 126.4 |
H6B—C6—H6C | 109.5 | C28—C29—N24 | 105.85 (17) |
N5—C7—C8 | 110.86 (18) | C28—C29—C30 | 130.62 (19) |
N5—C7—C6 | 121.8 (2) | N24—C29—C30 | 123.50 (18) |
C8—C7—C6 | 127.4 (2) | C29—C30—H30A | 109.5 |
C9—C8—C7 | 106.54 (17) | C29—C30—H30B | 109.5 |
C9—C8—H8 | 126.7 | H30A—C30—H30B | 109.5 |
C7—C8—H8 | 126.7 | C29—C30—H30C | 109.5 |
N6—C9—C8 | 106.00 (17) | H30A—C30—H30C | 109.5 |
N6—C9—C10 | 123.29 (18) | H30B—C30—H30C | 109.5 |
C8—C9—C10 | 130.71 (18) | C32—C31—H31A | 109.5 |
C9—C10—H10A | 109.5 | C32—C31—H31B | 109.5 |
C9—C10—H10B | 109.5 | H31A—C31—H31B | 109.5 |
H10A—C10—H10B | 109.5 | C32—C31—H31C | 109.5 |
C9—C10—H10C | 109.5 | H31A—C31—H31C | 109.5 |
H10A—C10—H10C | 109.5 | H31B—C31—H31C | 109.5 |
H10B—C10—H10C | 109.5 | N25—C32—C33 | 110.11 (18) |
C12—C11—H11A | 109.5 | N25—C32—C31 | 122.51 (19) |
C12—C11—H11B | 109.5 | C33—C32—C31 | 127.37 (19) |
H11A—C11—H11B | 109.5 | C34—C33—C32 | 107.23 (18) |
C12—C11—H11C | 109.5 | C34—C33—H33 | 126.4 |
H11A—C11—H11C | 109.5 | C32—C33—H33 | 126.4 |
H11B—C11—H11C | 109.5 | C33—C34—N26 | 105.99 (18) |
N3—C12—C13 | 110.37 (18) | C33—C34—C35 | 131.2 (2) |
N3—C12—C11 | 121.8 (2) | N26—C34—C35 | 122.7 (2) |
C13—C12—C11 | 127.8 (2) | C34—C35—H35A | 109.5 |
C14—C13—C12 | 107.14 (18) | C34—C35—H35B | 109.5 |
C14—C13—H13 | 126.4 | H35A—C35—H35B | 109.5 |
C12—C13—H13 | 126.4 | C34—C35—H35C | 109.5 |
N4—C14—C13 | 105.48 (17) | H35A—C35—H35C | 109.5 |
N4—C14—C15 | 122.54 (19) | H35B—C35—H35C | 109.5 |
C13—C14—C15 | 131.97 (19) | N22ii—C36—N26 | 110.62 (14) |
C14—C15—H15A | 109.5 | N22ii—C36—N24ii | 111.74 (14) |
C14—C15—H15B | 109.5 | N26—C36—N24ii | 110.34 (15) |
H15A—C15—H15B | 109.5 | N22ii—C36—H36 | 108.0 |
C14—C15—H15C | 109.5 | N26—C36—H36 | 108.0 |
H15A—C15—H15C | 109.5 | N24ii—C36—H36 | 108.0 |
H15B—C15—H15C | 109.5 | Cl4—Ni3—Cl1 | 107.78 (3) |
N2i—C16—N4 | 110.57 (14) | Cl4—Ni3—Cl3 | 108.01 (2) |
N2i—C16—N6 | 111.44 (14) | Cl1—Ni3—Cl3 | 109.46 (3) |
N4—C16—N6 | 111.57 (14) | Cl4—Ni3—Cl2 | 106.58 (3) |
N2i—C16—H16 | 107.7 | Cl1—Ni3—Cl2 | 117.42 (3) |
N4—C16—H16 | 107.7 | Cl3—Ni3—Cl2 | 107.24 (3) |
N6—C16—H16 | 107.7 | O97—C97—H97A | 109.5 |
N21—Ni2—N21ii | 180 | O97—C97—H97B | 109.5 |
N21—Ni2—N23ii | 94.60 (6) | H97A—C97—H97B | 109.5 |
N21ii—Ni2—N23ii | 85.40 (6) | O97—C97—H97C | 109.5 |
N21—Ni2—N23 | 85.39 (6) | H97A—C97—H97C | 109.5 |
N21ii—Ni2—N23 | 94.61 (6) | H97B—C97—H97C | 109.5 |
N23ii—Ni2—N23 | 180 | C97—O97—H97D | 109.5 |
N21—Ni2—N25 | 94.74 (6) | ||
N3—Ni1—N1—C2 | 43.6 (2) | C9—N6—C16—N4 | 122.73 (18) |
N3i—Ni1—N1—C2 | −136.4 (2) | N5—N6—C16—N4 | −61.0 (2) |
N5i—Ni1—N1—C2 | 137.7 (2) | N23ii—Ni2—N21—C22 | −41.2 (2) |
N5—Ni1—N1—C2 | −42.3 (2) | N23—Ni2—N21—C22 | 138.8 (2) |
N3—Ni1—N1—N2 | −136.12 (13) | N25—Ni2—N21—C22 | 45.5 (2) |
N3i—Ni1—N1—N2 | 43.88 (13) | N25ii—Ni2—N21—C22 | −134.5 (2) |
N5i—Ni1—N1—N2 | −41.98 (13) | N23ii—Ni2—N21—N22 | 134.82 (13) |
N5—Ni1—N1—N2 | 138.03 (13) | N23—Ni2—N21—N22 | −45.18 (13) |
C2—N1—N2—C4 | −0.2 (2) | N25—Ni2—N21—N22 | −138.54 (13) |
Ni1—N1—N2—C4 | 179.54 (12) | N25ii—Ni2—N21—N22 | 41.46 (13) |
C2—N1—N2—C16i | 179.16 (17) | C22—N21—N22—C24 | 0.0 (2) |
Ni1—N1—N2—C16i | −1.1 (2) | Ni2—N21—N22—C24 | −177.25 (12) |
N1i—Ni1—N3—C12 | −133.9 (2) | C22—N21—N22—C36ii | −178.72 (16) |
N1—Ni1—N3—C12 | 46.1 (2) | Ni2—N21—N22—C36ii | 4.0 (2) |
N5i—Ni1—N3—C12 | −40.4 (2) | N21—Ni2—N23—C27 | −134.8 (2) |
N5—Ni1—N3—C12 | 139.6 (2) | N21ii—Ni2—N23—C27 | 45.2 (2) |
N1i—Ni1—N3—N4 | 42.24 (13) | N25—Ni2—N23—C27 | −40.3 (2) |
N1—Ni1—N3—N4 | −137.76 (13) | N25ii—Ni2—N23—C27 | 139.7 (2) |
N5i—Ni1—N3—N4 | 135.66 (13) | N21—Ni2—N23—N24 | 42.61 (13) |
N5—Ni1—N3—N4 | −44.34 (13) | N21ii—Ni2—N23—N24 | −137.39 (13) |
C12—N3—N4—C14 | 0.2 (2) | N25—Ni2—N23—N24 | 137.07 (13) |
Ni1—N3—N4—C14 | −177.12 (12) | N25ii—Ni2—N23—N24 | −42.93 (13) |
C12—N3—N4—C16 | 179.07 (16) | C27—N23—N24—C29 | −0.6 (2) |
Ni1—N3—N4—C16 | 1.7 (2) | Ni2—N23—N24—C29 | −178.77 (12) |
N3—Ni1—N5—C7 | −140.3 (2) | C27—N23—N24—C36ii | 179.35 (16) |
N3i—Ni1—N5—C7 | 39.7 (2) | Ni2—N23—N24—C36ii | 1.1 (2) |
N1i—Ni1—N5—C7 | 133.7 (2) | N21—Ni2—N25—C32 | 36.7 (2) |
N1—Ni1—N5—C7 | −46.3 (2) | N21ii—Ni2—N25—C32 | −143.3 (2) |
N3—Ni1—N5—N6 | 44.03 (12) | N23ii—Ni2—N25—C32 | 131.0 (2) |
N3i—Ni1—N5—N6 | −135.97 (12) | N23—Ni2—N25—C32 | −49.0 (2) |
N1i—Ni1—N5—N6 | −41.99 (12) | N21—Ni2—N25—N26 | −133.78 (13) |
N1—Ni1—N5—N6 | 138.01 (12) | N21ii—Ni2—N25—N26 | 46.22 (13) |
C7—N5—N6—C9 | −1.1 (2) | N23ii—Ni2—N25—N26 | −39.46 (13) |
Ni1—N5—N6—C9 | 175.94 (12) | N23—Ni2—N25—N26 | 140.54 (13) |
C7—N5—N6—C16 | −177.99 (16) | C32—N25—N26—C34 | −1.0 (2) |
Ni1—N5—N6—C16 | −0.90 (19) | Ni2—N25—N26—C34 | 172.49 (13) |
N2—N1—C2—C3 | 0.6 (2) | C32—N25—N26—C36 | −178.77 (16) |
Ni1—N1—C2—C3 | −179.13 (16) | Ni2—N25—N26—C36 | −5.3 (2) |
N2—N1—C2—C1 | −178.3 (2) | N22—N21—C22—C23 | 0.4 (2) |
Ni1—N1—C2—C1 | 2.0 (4) | Ni2—N21—C22—C23 | 176.63 (15) |
N1—C2—C3—C4 | −0.7 (3) | N22—N21—C22—C21 | −179.50 (19) |
C1—C2—C3—C4 | 178.1 (2) | Ni2—N21—C22—C21 | −3.2 (3) |
N1—N2—C4—C3 | −0.2 (2) | N21—C22—C23—C24 | −0.6 (2) |
C16i—N2—C4—C3 | −179.51 (18) | C21—C22—C23—C24 | 179.3 (2) |
N1—N2—C4—C5 | 179.40 (19) | N21—N22—C24—C23 | −0.3 (2) |
C16i—N2—C4—C5 | 0.1 (3) | C36ii—N22—C24—C23 | 178.23 (17) |
C2—C3—C4—N2 | 0.5 (2) | N21—N22—C24—C25 | 179.31 (19) |
C2—C3—C4—C5 | −179.0 (2) | C36ii—N22—C24—C25 | −2.1 (3) |
N6—N5—C7—C8 | 1.1 (2) | C22—C23—C24—N22 | 0.5 (2) |
Ni1—N5—C7—C8 | −174.92 (15) | C22—C23—C24—C25 | −179.1 (2) |
N6—N5—C7—C6 | −178.7 (2) | N24—N23—C27—C28 | 0.3 (2) |
Ni1—N5—C7—C6 | 5.3 (4) | Ni2—N23—C27—C28 | 177.90 (15) |
N5—C7—C8—C9 | −0.7 (2) | N24—N23—C27—C26 | −178.92 (19) |
C6—C7—C8—C9 | 179.1 (2) | Ni2—N23—C27—C26 | −1.3 (3) |
N5—N6—C9—C8 | 0.8 (2) | N23—C27—C28—C29 | 0.1 (2) |
C16—N6—C9—C8 | 177.22 (17) | C26—C27—C28—C29 | 179.2 (2) |
N5—N6—C9—C10 | −179.96 (18) | C27—C28—C29—N24 | −0.4 (2) |
C16—N6—C9—C10 | −3.5 (3) | C27—C28—C29—C30 | −178.4 (2) |
C7—C8—C9—N6 | −0.1 (2) | N23—N24—C29—C28 | 0.6 (2) |
C7—C8—C9—C10 | −179.3 (2) | C36ii—N24—C29—C28 | −179.29 (18) |
N4—N3—C12—C13 | 0.1 (2) | N23—N24—C29—C30 | 178.81 (19) |
Ni1—N3—C12—C13 | 176.51 (17) | C36ii—N24—C29—C30 | −1.1 (3) |
N4—N3—C12—C11 | −179.9 (2) | N26—N25—C32—C33 | 0.9 (2) |
Ni1—N3—C12—C11 | −3.5 (4) | Ni2—N25—C32—C33 | −170.26 (16) |
N3—C12—C13—C14 | −0.4 (3) | N26—N25—C32—C31 | −179.7 (2) |
C11—C12—C13—C14 | 179.6 (2) | Ni2—N25—C32—C31 | 9.1 (4) |
N3—N4—C14—C13 | −0.5 (2) | N25—C32—C33—C34 | −0.5 (3) |
C16—N4—C14—C13 | −179.21 (18) | C31—C32—C33—C34 | −179.9 (2) |
N3—N4—C14—C15 | −179.27 (19) | C32—C33—C34—N26 | −0.1 (3) |
C16—N4—C14—C15 | 2.0 (3) | C32—C33—C34—C35 | 177.6 (3) |
C12—C13—C14—N4 | 0.5 (2) | N25—N26—C34—C33 | 0.7 (2) |
C12—C13—C14—C15 | 179.2 (2) | C36—N26—C34—C33 | 178.20 (19) |
C14—N4—C16—N2i | 115.04 (19) | N25—N26—C34—C35 | −177.3 (2) |
N3—N4—C16—N2i | −63.6 (2) | C36—N26—C34—C35 | 0.2 (3) |
C14—N4—C16—N6 | −120.34 (19) | C34—N26—C36—N22ii | 124.1 (2) |
N3—N4—C16—N6 | 61.0 (2) | N25—N26—C36—N22ii | −58.5 (2) |
C9—N6—C16—N2i | −113.14 (19) | C34—N26—C36—N24ii | −111.7 (2) |
N5—N6—C16—N2i | 63.10 (19) | N25—N26—C36—N24ii | 65.7 (2) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+2, −y+1, −z. |