Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806017570/ac2009sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806017570/ac2009Isup2.hkl |
CCDC reference: 610673
Data collection: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXTL (Bruker, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Ni(C2H8N2)3]Cl2·2H2O | F(000) = 2208.0 |
Mr = 345.93 | Dx = 1.471 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: C -2yc | Cell parameters from 1679 reflections |
a = 26.186 (2) Å | θ = 1.4–23.7° |
b = 13.8917 (9) Å | µ = 1.59 mm−1 |
c = 12.8986 (8) Å | T = 293 K |
β = 93.197 (2)° | Block, colourless |
V = 4684.8 (6) Å3 | 0.30 × 0.30 × 0.30 mm |
Z = 12 |
Bruker SMART CCD area detector diffractometer | 5282 independent reflections |
Radiation source: fine-focus sealed tube | 4247 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
φ and ω scans | θmax = 25.3°, θmin = 1.6° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −22→31 |
Tmin = 0.627, Tmax = 0.627 | k = −16→15 |
12308 measured reflections | l = −15→15 |
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)] = 0.034 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.099 | w = 1/[σ2(Fo2) + (0.0519P)2 + 4.1952P] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max < 0.001 |
4247 reflections | Δρmax = 0.80 e Å−3 |
486 parameters | Δρmin = −0.45 e Å−3 |
20 restraints | Absolute structure: Flack (1983), with how many Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.00 (2) |
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 | 0.250270 (17) | 0.77240 (6) | 0.51366 (3) | 0.0263 (3) | |
Ni2 | 0.41627 (3) | 0.72688 (4) | 0.99565 (9) | 0.02602 (18) | |
Ni3 | 0.58250 (3) | 0.77185 (4) | 0.49404 (7) | 0.02559 (19) | |
O1 | 0.2484 (2) | 0.6837 (3) | 0.0442 (4) | 0.0548 (15) | |
O2 | 0.2536 (2) | 0.6103 (4) | 0.2479 (4) | 0.0593 (14) | |
O6 | 0.5860 (2) | 0.3156 (4) | 0.4579 (4) | 0.0565 (14)* | |
O3 | 0.4103 (2) | 0.1064 (4) | 0.7575 (4) | 0.0671 (15) | |
O4 | 0.4181 (2) | 0.1825 (3) | 0.9599 (4) | 0.0576 (13) | |
O5 | 0.5874 (2) | 0.3926 (5) | 0.2618 (4) | 0.0653 (14)* | |
C13 | 0.5556 (3) | 0.5679 (5) | 0.4823 (7) | 0.044 (2) | |
H13A | 0.5436 | 0.5126 | 0.4420 | 0.052* | |
H13B | 0.5418 | 0.5638 | 0.5503 | 0.052* | |
C14 | 0.6128 (3) | 0.5668 (5) | 0.4932 (6) | 0.0378 (18) | |
H14A | 0.6246 | 0.5102 | 0.5315 | 0.045* | |
H14B | 0.6269 | 0.5654 | 0.4253 | 0.045* | |
C3 | 0.2789 (3) | 0.8624 (7) | 0.3198 (7) | 0.046 (2) | |
H3A | 0.2895 | 0.8558 | 0.2493 | 0.056* | |
H3B | 0.2940 | 0.9207 | 0.3491 | 0.056* | |
C4 | 0.2215 (3) | 0.8694 (7) | 0.3186 (6) | 0.050 (2) | |
H4A | 0.2100 | 0.9265 | 0.2810 | 0.059* | |
H4B | 0.2062 | 0.8136 | 0.2839 | 0.059* | |
C11 | 0.4461 (3) | 0.9311 (5) | 0.9974 (6) | 0.0370 (17) | |
H11A | 0.4618 | 0.9315 | 0.9311 | 0.044* | |
H11B | 0.4572 | 0.9882 | 1.0357 | 0.044* | |
C12 | 0.3892 (3) | 0.9309 (5) | 0.9808 (7) | 0.044 (2) | |
H12A | 0.3737 | 0.9359 | 1.0471 | 0.052* | |
H12B | 0.3783 | 0.9858 | 0.9388 | 0.052* | |
C7 | 0.4421 (3) | 0.6312 (7) | 1.1944 (6) | 0.0446 (19) | |
H7A | 0.4573 | 0.6879 | 1.2273 | 0.053* | |
H7B | 0.4531 | 0.5752 | 1.2347 | 0.053* | |
C8 | 0.3841 (3) | 0.6390 (6) | 1.1903 (7) | 0.049 (2) | |
H8A | 0.3687 | 0.5812 | 1.1600 | 0.059* | |
H8B | 0.3722 | 0.6469 | 1.2597 | 0.059* | |
C9 | 0.4496 (3) | 0.6276 (6) | 0.8094 (6) | 0.0452 (19) | |
H9A | 0.4647 | 0.5712 | 0.8431 | 0.054* | |
H9B | 0.4616 | 0.6314 | 0.7397 | 0.054* | |
C10 | 0.3920 (3) | 0.6196 (7) | 0.8046 (6) | 0.0446 (18) | |
H10A | 0.3771 | 0.6734 | 0.7657 | 0.053* | |
H10B | 0.3815 | 0.5606 | 0.7692 | 0.053* | |
C15 | 0.6165 (3) | 0.8667 (6) | 0.6901 (6) | 0.046 (2) | |
H15A | 0.6291 | 0.9227 | 0.7283 | 0.056* | |
H15B | 0.6322 | 0.8097 | 0.7213 | 0.056* | |
C16 | 0.5593 (3) | 0.8606 (7) | 0.6931 (7) | 0.056 (2) | |
H16A | 0.5497 | 0.8536 | 0.7643 | 0.068* | |
H16B | 0.5437 | 0.9189 | 0.6647 | 0.068* | |
C17 | 0.6066 (3) | 0.8735 (7) | 0.3020 (6) | 0.047 (2) | |
H17A | 0.6152 | 0.8699 | 0.2300 | 0.057* | |
H17B | 0.6225 | 0.9306 | 0.3326 | 0.057* | |
C18 | 0.5487 (3) | 0.8796 (7) | 0.3081 (6) | 0.0505 (19) | |
H18A | 0.5360 | 0.9385 | 0.2755 | 0.061* | |
H18B | 0.5325 | 0.8255 | 0.2717 | 0.061* | |
C1 | 0.2790 (3) | 0.8784 (7) | 0.7042 (6) | 0.048 (2) | |
H1A | 0.2909 | 0.9363 | 0.7399 | 0.057* | |
H1B | 0.2937 | 0.8231 | 0.7409 | 0.057* | |
C2 | 0.2212 (3) | 0.8734 (8) | 0.7008 (7) | 0.050 (2) | |
H2A | 0.2095 | 0.8723 | 0.7708 | 0.060* | |
H2B | 0.2067 | 0.9294 | 0.6653 | 0.060* | |
C5 | 0.2221 (3) | 0.5693 (5) | 0.5148 (6) | 0.041 (2) | |
H5A | 0.2104 | 0.5116 | 0.4784 | 0.049* | |
H6B | 0.2070 | 0.5707 | 0.5817 | 0.049* | |
C6 | 0.2801 (3) | 0.5674 (5) | 0.5305 (6) | 0.0343 (18) | |
H6A | 0.2907 | 0.5135 | 0.5745 | 0.041* | |
H5B | 0.2954 | 0.5598 | 0.4642 | 0.041* | |
Cl1 | 0.25234 (8) | 0.09788 (16) | 0.50712 (17) | 0.0516 (6) | |
Cl5 | 0.58309 (10) | 0.09717 (9) | 0.4979 (2) | 0.0473 (4) | |
Cl4 | 0.41631 (11) | 0.59980 (9) | 0.4993 (2) | 0.0506 (3) | |
Cl2 | 0.24875 (10) | 0.38611 (15) | 0.31461 (16) | 0.0469 (4) | |
Cl3 | 0.42028 (8) | 0.11590 (14) | 1.19457 (14) | 0.0523 (4) | |
Cl6 | 0.58160 (8) | 0.61568 (14) | 0.19103 (14) | 0.0472 (4) | |
N13 | 0.5376 (2) | 0.6572 (4) | 0.4301 (4) | 0.0282 (13) | |
HA13 | 0.5043 | 0.6671 | 0.4407 | 0.034* | |
HB13 | 0.5412 | 0.6530 | 0.3612 | 0.034* | |
N14 | 0.6294 (2) | 0.6548 (4) | 0.5494 (5) | 0.0350 (14) | |
HA14 | 0.6624 | 0.6672 | 0.5386 | 0.042* | |
HB14 | 0.6263 | 0.6468 | 0.6180 | 0.042* | |
N3 | 0.2967 (2) | 0.7787 (4) | 0.3819 (5) | 0.0343 (15) | |
HA3 | 0.3299 | 0.7858 | 0.4028 | 0.041* | |
HB3 | 0.2932 | 0.7244 | 0.3443 | 0.041* | |
N4 | 0.2057 (2) | 0.8740 (5) | 0.4252 (5) | 0.0364 (15) | |
HA4 | 0.1722 | 0.8598 | 0.4273 | 0.044* | |
HB4 | 0.2109 | 0.9336 | 0.4511 | 0.044* | |
N11 | 0.4615 (2) | 0.8440 (4) | 1.0564 (5) | 0.0356 (15) | |
HA11 | 0.4563 | 0.8523 | 1.1242 | 0.043* | |
HB11 | 0.4949 | 0.8318 | 1.0498 | 0.043* | |
N12 | 0.3724 (2) | 0.8406 (4) | 0.9280 (4) | 0.0298 (13) | |
HA12 | 0.3773 | 0.8445 | 0.8596 | 0.036* | |
HB12 | 0.3389 | 0.8304 | 0.9361 | 0.036* | |
N7 | 0.4584 (2) | 0.6225 (5) | 1.0874 (4) | 0.0390 (15) | |
HA7 | 0.4518 | 0.5629 | 1.0628 | 0.047* | |
HB7 | 0.4921 | 0.6337 | 1.0856 | 0.047* | |
N8 | 0.3699 (3) | 0.7230 (4) | 1.1261 (5) | 0.0409 (17) | |
HA8 | 0.3745 | 0.7772 | 1.1637 | 0.049* | |
HB8 | 0.3367 | 0.7193 | 1.1044 | 0.049* | |
N9 | 0.4648 (2) | 0.7148 (4) | 0.8684 (5) | 0.0335 (14) | |
HA9 | 0.4613 | 0.7671 | 0.8273 | 0.040* | |
HB9 | 0.4977 | 0.7104 | 0.8920 | 0.040* | |
N10 | 0.3737 (2) | 0.6194 (5) | 0.9115 (4) | 0.0363 (14) | |
HA10 | 0.3788 | 0.5614 | 0.9413 | 0.044* | |
HB10 | 0.3400 | 0.6329 | 0.9101 | 0.044* | |
N15 | 0.6291 (2) | 0.8743 (5) | 0.5784 (5) | 0.0390 (15) | |
HA15 | 0.6624 | 0.8613 | 0.5715 | 0.047* | |
HB15 | 0.6226 | 0.9341 | 0.5543 | 0.047* | |
N16 | 0.5416 (3) | 0.7776 (5) | 0.6320 (5) | 0.0403 (17) | |
HB16 | 0.5079 | 0.7828 | 0.6157 | 0.048* | |
HA16 | 0.5470 | 0.7233 | 0.6690 | 0.048* | |
N17 | 0.6256 (2) | 0.7865 (4) | 0.3588 (5) | 0.0350 (15) | |
HA17 | 0.6591 | 0.7929 | 0.3772 | 0.042* | |
HB17 | 0.6215 | 0.7341 | 0.3182 | 0.042* | |
N18 | 0.5361 (2) | 0.8780 (5) | 0.4180 (5) | 0.0373 (14) | |
HA18 | 0.5028 | 0.8638 | 0.4233 | 0.045* | |
HB18 | 0.5423 | 0.9360 | 0.4471 | 0.045* | |
N1 | 0.2945 (2) | 0.8791 (5) | 0.5964 (5) | 0.0392 (15) | |
HB1 | 0.3280 | 0.8658 | 0.5944 | 0.047* | |
HA1 | 0.2886 | 0.9375 | 0.5677 | 0.047* | |
N2 | 0.2053 (3) | 0.7858 (5) | 0.6456 (5) | 0.0387 (16) | |
HB2 | 0.1719 | 0.7893 | 0.6253 | 0.046* | |
HA2 | 0.2100 | 0.7343 | 0.6873 | 0.046* | |
N6 | 0.2969 (2) | 0.6580 (5) | 0.5792 (5) | 0.0391 (16) | |
HA6 | 0.3300 | 0.6689 | 0.5677 | 0.047* | |
HB6 | 0.2938 | 0.6550 | 0.6483 | 0.047* | |
N5 | 0.2060 (2) | 0.6547 (4) | 0.4543 (5) | 0.0325 (14) | |
HB5 | 0.1725 | 0.6661 | 0.4607 | 0.039* | |
HA5 | 0.2113 | 0.6456 | 0.3867 | 0.039* | |
H1E | 0.243 (2) | 0.672 (3) | −0.0202 (17) | 0.039* | |
H1F | 0.2352 (16) | 0.7380 (19) | 0.057 (3) | 0.039* | |
H2E | 0.252 (2) | 0.632 (2) | 0.186 (2) | 0.039* | |
H2F | 0.251 (2) | 0.5495 (14) | 0.244 (3) | 0.039* | |
H6E | 0.5555 (9) | 0.308 (3) | 0.433 (3) | 0.039* | |
H6F | 0.5847 (18) | 0.340 (3) | 0.518 (2) | 0.039* | |
H3E | 0.4091 (17) | 0.131 (2) | 0.6969 (19) | 0.039* | |
H3F | 0.415 (2) | 0.0462 (14) | 0.751 (3) | 0.039* | |
H4E | 0.4367 (12) | 0.196 (4) | 1.014 (3) | 0.039* | |
H4F | 0.3874 (8) | 0.197 (4) | 0.972 (3) | 0.039* | |
H5E | 0.5686 (14) | 0.442 (2) | 0.251 (3) | 0.039* | |
H5F | 0.6025 (16) | 0.399 (3) | 0.321 (2) | 0.039* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0256 (4) | 0.0273 (5) | 0.0260 (6) | −0.0006 (3) | 0.0011 (5) | 0.0004 (3) |
Ni2 | 0.0249 (3) | 0.0265 (3) | 0.0265 (4) | 0.0010 (4) | −0.0002 (3) | −0.0002 (3) |
Ni3 | 0.0257 (3) | 0.0251 (3) | 0.0260 (5) | −0.0007 (4) | 0.0013 (3) | −0.0003 (3) |
O1 | 0.102 (4) | 0.034 (2) | 0.028 (2) | −0.001 (2) | 0.006 (2) | 0.0046 (15) |
O2 | 0.096 (4) | 0.048 (2) | 0.034 (2) | −0.004 (2) | 0.007 (2) | −0.0107 (18) |
O3 | 0.102 (4) | 0.061 (3) | 0.039 (2) | 0.008 (3) | 0.005 (3) | 0.006 (2) |
O4 | 0.066 (3) | 0.055 (3) | 0.051 (2) | −0.001 (2) | −0.002 (2) | −0.0054 (19) |
C13 | 0.060 (5) | 0.023 (3) | 0.048 (4) | −0.008 (3) | 0.003 (4) | −0.004 (3) |
C14 | 0.024 (4) | 0.036 (4) | 0.053 (5) | 0.005 (3) | 0.005 (3) | −0.007 (3) |
C3 | 0.055 (4) | 0.052 (5) | 0.033 (4) | −0.003 (4) | 0.010 (3) | 0.015 (3) |
C4 | 0.065 (5) | 0.045 (5) | 0.038 (4) | 0.006 (4) | −0.003 (4) | 0.010 (4) |
C11 | 0.031 (4) | 0.035 (3) | 0.045 (4) | −0.003 (3) | 0.007 (3) | 0.001 (3) |
C12 | 0.061 (5) | 0.022 (3) | 0.048 (4) | 0.008 (3) | 0.001 (4) | 0.004 (3) |
C7 | 0.047 (4) | 0.049 (4) | 0.037 (4) | −0.001 (4) | −0.007 (3) | 0.011 (3) |
C8 | 0.048 (4) | 0.051 (5) | 0.048 (4) | −0.005 (4) | 0.009 (4) | 0.016 (4) |
C9 | 0.051 (4) | 0.044 (4) | 0.041 (4) | 0.006 (3) | 0.007 (3) | −0.012 (3) |
C10 | 0.051 (4) | 0.044 (4) | 0.038 (4) | −0.002 (4) | −0.005 (3) | −0.012 (3) |
C15 | 0.055 (4) | 0.049 (4) | 0.035 (4) | 0.007 (4) | −0.009 (3) | −0.011 (3) |
C16 | 0.067 (5) | 0.058 (6) | 0.046 (4) | 0.006 (4) | 0.009 (4) | −0.014 (4) |
C17 | 0.063 (5) | 0.042 (4) | 0.037 (4) | −0.013 (4) | 0.008 (3) | 0.012 (3) |
C18 | 0.064 (5) | 0.046 (4) | 0.040 (4) | 0.007 (4) | −0.006 (3) | 0.011 (4) |
C1 | 0.055 (5) | 0.048 (5) | 0.039 (4) | −0.004 (4) | −0.011 (4) | −0.012 (4) |
C2 | 0.050 (5) | 0.062 (5) | 0.038 (4) | 0.011 (4) | 0.004 (3) | −0.014 (4) |
C5 | 0.057 (5) | 0.022 (3) | 0.045 (4) | −0.005 (3) | 0.011 (4) | −0.005 (3) |
C6 | 0.027 (4) | 0.035 (4) | 0.041 (4) | 0.005 (3) | 0.006 (3) | −0.001 (3) |
Cl1 | 0.0435 (11) | 0.0396 (12) | 0.0723 (16) | 0.0018 (11) | 0.0099 (10) | 0.0035 (10) |
Cl5 | 0.0406 (7) | 0.0359 (7) | 0.0659 (10) | −0.0015 (12) | 0.0073 (6) | 0.0008 (12) |
Cl4 | 0.0456 (7) | 0.0365 (6) | 0.0710 (9) | −0.0010 (13) | 0.0146 (6) | 0.0018 (13) |
Cl2 | 0.0541 (10) | 0.0507 (9) | 0.0360 (9) | −0.0059 (11) | 0.0030 (8) | −0.0078 (10) |
Cl3 | 0.0578 (9) | 0.0585 (9) | 0.0405 (8) | −0.0075 (9) | 0.0034 (8) | −0.0090 (9) |
Cl6 | 0.0509 (9) | 0.0532 (9) | 0.0373 (8) | −0.0048 (9) | 0.0005 (7) | −0.0080 (9) |
N13 | 0.026 (3) | 0.031 (3) | 0.027 (3) | −0.003 (2) | 0.000 (2) | −0.004 (2) |
N14 | 0.031 (3) | 0.037 (3) | 0.037 (3) | 0.001 (2) | −0.001 (2) | −0.001 (2) |
N3 | 0.029 (3) | 0.036 (3) | 0.038 (4) | −0.003 (2) | 0.005 (2) | −0.001 (2) |
N4 | 0.033 (3) | 0.035 (4) | 0.041 (3) | 0.000 (3) | 0.000 (2) | −0.001 (3) |
N11 | 0.031 (3) | 0.039 (3) | 0.036 (3) | −0.004 (2) | 0.002 (2) | −0.002 (2) |
N12 | 0.028 (3) | 0.035 (3) | 0.027 (3) | 0.001 (2) | 0.001 (2) | 0.006 (2) |
N7 | 0.038 (3) | 0.032 (3) | 0.047 (4) | 0.004 (3) | −0.003 (3) | 0.005 (3) |
N8 | 0.041 (4) | 0.050 (4) | 0.033 (3) | 0.002 (3) | 0.004 (3) | 0.004 (2) |
N9 | 0.028 (3) | 0.037 (3) | 0.037 (3) | 0.001 (2) | 0.006 (2) | 0.003 (2) |
N10 | 0.032 (3) | 0.037 (3) | 0.039 (3) | 0.000 (3) | −0.005 (2) | −0.003 (3) |
N15 | 0.041 (3) | 0.032 (3) | 0.044 (3) | −0.006 (3) | 0.000 (3) | −0.006 (3) |
N16 | 0.043 (4) | 0.049 (4) | 0.030 (3) | 0.005 (3) | 0.008 (3) | 0.003 (2) |
N17 | 0.032 (3) | 0.037 (3) | 0.037 (4) | −0.005 (3) | 0.007 (3) | −0.004 (2) |
N18 | 0.035 (3) | 0.033 (3) | 0.044 (3) | 0.000 (3) | −0.003 (2) | 0.002 (3) |
N1 | 0.037 (3) | 0.033 (3) | 0.048 (4) | −0.005 (3) | −0.002 (3) | 0.000 (3) |
N2 | 0.042 (4) | 0.046 (4) | 0.029 (3) | 0.006 (3) | 0.002 (3) | −0.002 (3) |
N6 | 0.035 (3) | 0.044 (4) | 0.038 (4) | 0.006 (3) | 0.003 (3) | 0.004 (3) |
N5 | 0.032 (3) | 0.034 (3) | 0.032 (3) | −0.003 (2) | 0.003 (2) | −0.006 (2) |
Ni1—N5 | 2.122 (6) | C15—N15 | 1.500 (11) |
Ni1—N4 | 2.123 (6) | C15—C16 | 1.502 (12) |
Ni1—N1 | 2.130 (6) | C15—H15A | 0.9700 |
Ni1—N2 | 2.131 (7) | C15—H15B | 0.9700 |
Ni1—N3 | 2.146 (6) | C16—N16 | 1.457 (11) |
Ni1—N6 | 2.149 (6) | C16—H16A | 0.9700 |
Ni2—N12 | 2.114 (5) | C16—H16B | 0.9700 |
Ni2—N10 | 2.125 (6) | C17—N17 | 1.485 (10) |
Ni2—N8 | 2.130 (7) | C17—C18 | 1.525 (12) |
Ni2—N11 | 2.135 (6) | C17—H17A | 0.9700 |
Ni2—N9 | 2.137 (6) | C17—H17B | 0.9700 |
Ni2—N7 | 2.138 (6) | C18—N18 | 1.472 (10) |
Ni3—N18 | 2.116 (6) | C18—H18A | 0.9700 |
Ni3—N13 | 2.119 (5) | C18—H18B | 0.9700 |
Ni3—N16 | 2.129 (7) | C1—N1 | 1.469 (10) |
Ni3—N15 | 2.133 (6) | C1—C2 | 1.513 (10) |
Ni3—N14 | 2.136 (6) | C1—H1A | 0.9700 |
Ni3—N17 | 2.140 (6) | C1—H1B | 0.9700 |
O1—H1E | 0.850 (19) | C2—N2 | 1.460 (11) |
O1—H1F | 0.850 (18) | C2—H2A | 0.9700 |
O2—H2E | 0.850 (19) | C2—H2B | 0.9700 |
O2—H2F | 0.850 (18) | C5—N5 | 1.468 (9) |
O6—H6E | 0.850 (18) | C5—C6 | 1.520 (11) |
O6—H6F | 0.850 (19) | C5—H5A | 0.9700 |
O3—H3E | 0.850 (18) | C5—H6B | 0.9700 |
O3—H3F | 0.850 (18) | C6—N6 | 1.465 (9) |
O4—H4E | 0.850 (19) | C6—H6A | 0.9700 |
O4—H4F | 0.850 (19) | C6—H5B | 0.9700 |
O5—H5E | 0.850 (18) | N13—HA13 | 0.9000 |
O5—H5F | 0.850 (18) | N13—HB13 | 0.9000 |
C13—N13 | 1.476 (9) | N14—HA14 | 0.9000 |
C13—C14 | 1.497 (8) | N14—HB14 | 0.9000 |
C13—H13A | 0.9700 | N3—HA3 | 0.9000 |
C13—H13B | 0.9700 | N3—HB3 | 0.9000 |
C14—N14 | 1.473 (9) | N4—HA4 | 0.9000 |
C14—H14A | 0.9700 | N4—HB4 | 0.9000 |
C14—H14B | 0.9700 | N11—HA11 | 0.9000 |
C3—N3 | 1.473 (10) | N11—HB11 | 0.9000 |
C3—C4 | 1.504 (11) | N12—HA12 | 0.9000 |
C3—H3A | 0.9700 | N12—HB12 | 0.9000 |
C3—H3B | 0.9700 | N7—HA7 | 0.9000 |
C4—N4 | 1.459 (10) | N7—HB7 | 0.9000 |
C4—H4A | 0.9700 | N8—HA8 | 0.9000 |
C4—H4B | 0.9700 | N8—HB8 | 0.9000 |
C11—N11 | 1.475 (9) | N9—HA9 | 0.9000 |
C11—C12 | 1.494 (8) | N9—HB9 | 0.9000 |
C11—H11A | 0.9700 | N10—HA10 | 0.9000 |
C11—H11B | 0.9700 | N10—HB10 | 0.9000 |
C12—N12 | 1.482 (9) | N15—HA15 | 0.9000 |
C12—H12A | 0.9700 | N15—HB15 | 0.9000 |
C12—H12B | 0.9700 | N16—HB16 | 0.9000 |
C7—N7 | 1.473 (10) | N16—HA16 | 0.9000 |
C7—C8 | 1.521 (11) | N17—HA17 | 0.9000 |
C7—H7A | 0.9700 | N17—HB17 | 0.9000 |
C7—H7B | 0.9700 | N18—HA18 | 0.9000 |
C8—N8 | 1.467 (10) | N18—HB18 | 0.9000 |
C8—H8A | 0.9700 | N1—HB1 | 0.9000 |
C8—H8B | 0.9700 | N1—HA1 | 0.9000 |
C9—N9 | 1.474 (10) | N2—HB2 | 0.9000 |
C9—C10 | 1.508 (11) | N2—HA2 | 0.9000 |
C9—H9A | 0.9700 | N6—HA6 | 0.9000 |
C9—H9B | 0.9700 | N6—HB6 | 0.9000 |
C10—N10 | 1.486 (10) | N5—HB5 | 0.9000 |
C10—H10A | 0.9700 | N5—HA5 | 0.9000 |
C10—H10B | 0.9700 | ||
N5—Ni1—N4 | 92.6 (3) | H18A—C18—H18B | 108.3 |
N5—Ni1—N1 | 170.9 (2) | N1—C1—C2 | 107.5 (6) |
N4—Ni1—N1 | 94.2 (2) | N1—C1—H1A | 110.2 |
N5—Ni1—N2 | 92.3 (2) | C2—C1—H1A | 110.2 |
N4—Ni1—N2 | 93.4 (2) | N1—C1—H1B | 110.2 |
N1—Ni1—N2 | 81.3 (2) | C2—C1—H1B | 110.2 |
N5—Ni1—N3 | 93.9 (2) | H1A—C1—H1B | 108.5 |
N4—Ni1—N3 | 82.3 (2) | N2—C2—C1 | 108.1 (8) |
N1—Ni1—N3 | 93.0 (2) | N2—C2—H2A | 110.1 |
N2—Ni1—N3 | 172.6 (2) | C1—C2—H2A | 110.1 |
N5—Ni1—N6 | 81.9 (2) | N2—C2—H2B | 110.1 |
N4—Ni1—N6 | 170.6 (3) | C1—C2—H2B | 110.1 |
N1—Ni1—N6 | 92.1 (3) | H2A—C2—H2B | 108.4 |
N2—Ni1—N6 | 94.5 (3) | N5—C5—C6 | 109.9 (6) |
N3—Ni1—N6 | 90.4 (2) | N5—C5—H5A | 109.7 |
N12—Ni2—N10 | 93.2 (3) | C6—C5—H5A | 109.7 |
N12—Ni2—N8 | 91.4 (2) | N5—C5—H6B | 109.7 |
N10—Ni2—N8 | 94.6 (2) | C6—C5—H6B | 109.7 |
N12—Ni2—N11 | 81.95 (15) | H5A—C5—H6B | 108.2 |
N10—Ni2—N11 | 170.8 (2) | N6—C6—C5 | 108.5 (6) |
N8—Ni2—N11 | 93.3 (3) | N6—C6—H6A | 110.0 |
N12—Ni2—N9 | 94.2 (2) | C5—C6—H6A | 110.0 |
N10—Ni2—N9 | 82.5 (2) | N6—C6—H5B | 110.0 |
N8—Ni2—N9 | 173.82 (17) | C5—C6—H5B | 110.0 |
N11—Ni2—N9 | 90.0 (2) | H6A—C6—H5B | 108.4 |
N12—Ni2—N7 | 170.8 (2) | C13—N13—Ni3 | 107.3 (4) |
N10—Ni2—N7 | 92.65 (15) | C13—N13—HA13 | 110.3 |
N8—Ni2—N7 | 81.1 (2) | Ni3—N13—HA13 | 110.3 |
N11—Ni2—N7 | 93.2 (3) | C13—N13—HB13 | 110.3 |
N9—Ni2—N7 | 93.6 (2) | Ni3—N13—HB13 | 110.3 |
N18—Ni3—N13 | 92.9 (3) | HA13—N13—HB13 | 108.5 |
N18—Ni3—N16 | 93.4 (3) | C14—N14—Ni3 | 108.6 (4) |
N13—Ni3—N16 | 93.4 (2) | C14—N14—HA14 | 110.0 |
N18—Ni3—N15 | 93.95 (16) | Ni3—N14—HA14 | 110.0 |
N13—Ni3—N15 | 171.6 (3) | C14—N14—HB14 | 110.0 |
N16—Ni3—N15 | 81.3 (3) | Ni3—N14—HB14 | 110.0 |
N18—Ni3—N14 | 171.7 (2) | HA14—N14—HB14 | 108.3 |
N13—Ni3—N14 | 81.60 (15) | C3—N3—Ni1 | 106.7 (5) |
N16—Ni3—N14 | 93.2 (2) | C3—N3—HA3 | 110.4 |
N15—Ni3—N14 | 92.1 (3) | Ni1—N3—HA3 | 110.4 |
N18—Ni3—N17 | 82.6 (2) | C3—N3—HB3 | 110.4 |
N13—Ni3—N17 | 93.5 (2) | Ni1—N3—HB3 | 110.4 |
N16—Ni3—N17 | 172.18 (17) | HA3—N3—HB3 | 108.6 |
N15—Ni3—N17 | 92.2 (2) | C4—N4—Ni1 | 107.5 (5) |
N14—Ni3—N17 | 91.5 (2) | C4—N4—HA4 | 110.2 |
H1E—O1—H1F | 108 (2) | Ni1—N4—HA4 | 110.2 |
H2E—O2—H2F | 108 (2) | C4—N4—HB4 | 110.2 |
H6E—O6—H6F | 108 (2) | Ni1—N4—HB4 | 110.2 |
H3E—O3—H3F | 108 (2) | HA4—N4—HB4 | 108.5 |
H4E—O4—H4F | 108 (3) | C11—N11—Ni2 | 107.8 (4) |
H5E—O5—H5F | 108 (2) | C11—N11—HA11 | 110.1 |
N13—C13—C14 | 110.1 (7) | Ni2—N11—HA11 | 110.1 |
N13—C13—H13A | 109.6 | C11—N11—HB11 | 110.1 |
C14—C13—H13A | 109.6 | Ni2—N11—HB11 | 110.1 |
N13—C13—H13B | 109.6 | HA11—N11—HB11 | 108.5 |
C14—C13—H13B | 109.6 | C12—N12—Ni2 | 107.6 (4) |
H13A—C13—H13B | 108.2 | C12—N12—HA12 | 110.2 |
N14—C14—C13 | 107.7 (6) | Ni2—N12—HA12 | 110.2 |
N14—C14—H14A | 110.2 | C12—N12—HB12 | 110.2 |
C13—C14—H14A | 110.2 | Ni2—N12—HB12 | 110.2 |
N14—C14—H14B | 110.2 | HA12—N12—HB12 | 108.5 |
C13—C14—H14B | 110.2 | C7—N7—Ni2 | 107.2 (5) |
H14A—C14—H14B | 108.5 | C7—N7—HA7 | 110.3 |
N3—C3—C4 | 110.0 (7) | Ni2—N7—HA7 | 110.3 |
N3—C3—H3A | 109.7 | C7—N7—HB7 | 110.3 |
C4—C3—H3A | 109.7 | Ni2—N7—HB7 | 110.3 |
N3—C3—H3B | 109.7 | HA7—N7—HB7 | 108.5 |
C4—C3—H3B | 109.7 | C8—N8—Ni2 | 109.1 (5) |
H3A—C3—H3B | 108.2 | C8—N8—HA8 | 109.9 |
N4—C4—C3 | 109.2 (6) | Ni2—N8—HA8 | 109.9 |
N4—C4—H4A | 109.8 | C8—N8—HB8 | 109.9 |
C3—C4—H4A | 109.8 | Ni2—N8—HB8 | 109.9 |
N4—C4—H4B | 109.8 | HA8—N8—HB8 | 108.3 |
C3—C4—H4B | 109.8 | C9—N9—Ni2 | 107.8 (5) |
H4A—C4—H4B | 108.3 | C9—N9—HA9 | 110.1 |
N11—C11—C12 | 108.3 (6) | Ni2—N9—HA9 | 110.1 |
N11—C11—H11A | 110.0 | C9—N9—HB9 | 110.1 |
C12—C11—H11A | 110.0 | Ni2—N9—HB9 | 110.1 |
N11—C11—H11B | 110.0 | HA9—N9—HB9 | 108.5 |
C12—C11—H11B | 110.0 | C10—N10—Ni2 | 106.6 (5) |
H11A—C11—H11B | 108.4 | C10—N10—HA10 | 110.4 |
N12—C12—C11 | 109.6 (6) | Ni2—N10—HA10 | 110.4 |
N12—C12—H12A | 109.7 | C10—N10—HB10 | 110.4 |
C11—C12—H12A | 109.7 | Ni2—N10—HB10 | 110.4 |
N12—C12—H12B | 109.7 | HA10—N10—HB10 | 108.6 |
C11—C12—H12B | 109.7 | C15—N15—Ni3 | 107.0 (5) |
H12A—C12—H12B | 108.2 | C15—N15—HA15 | 110.3 |
N7—C7—C8 | 108.3 (6) | Ni3—N15—HA15 | 110.3 |
N7—C7—H7A | 110.0 | C15—N15—HB15 | 110.3 |
C8—C7—H7A | 110.0 | Ni3—N15—HB15 | 110.3 |
N7—C7—H7B | 110.0 | HA15—N15—HB15 | 108.6 |
C8—C7—H7B | 110.0 | C16—N16—Ni3 | 108.8 (5) |
H7A—C7—H7B | 108.4 | C16—N16—HB16 | 109.9 |
N8—C8—C7 | 107.3 (7) | Ni3—N16—HB16 | 109.9 |
N8—C8—H8A | 110.3 | C16—N16—HA16 | 109.9 |
C7—C8—H8A | 110.3 | Ni3—N16—HA16 | 109.9 |
N8—C8—H8B | 110.3 | HB16—N16—HA16 | 108.3 |
C7—C8—H8B | 110.3 | C17—N17—Ni3 | 107.6 (5) |
H8A—C8—H8B | 108.5 | C17—N17—HA17 | 110.2 |
N9—C9—C10 | 108.8 (7) | Ni3—N17—HA17 | 110.2 |
N9—C9—H9A | 109.9 | C17—N17—HB17 | 110.2 |
C10—C9—H9A | 109.9 | Ni3—N17—HB17 | 110.2 |
N9—C9—H9B | 109.9 | HA17—N17—HB17 | 108.5 |
C10—C9—H9B | 109.9 | C18—N18—Ni3 | 107.7 (5) |
H9A—C9—H9B | 108.3 | C18—N18—HA18 | 110.2 |
N10—C10—C9 | 109.6 (6) | Ni3—N18—HA18 | 110.2 |
N10—C10—H10A | 109.7 | C18—N18—HB18 | 110.2 |
C9—C10—H10A | 109.7 | Ni3—N18—HB18 | 110.2 |
N10—C10—H10B | 109.7 | HA18—N18—HB18 | 108.5 |
C9—C10—H10B | 109.7 | C1—N1—Ni1 | 107.4 (5) |
H10A—C10—H10B | 108.2 | C1—N1—HB1 | 110.2 |
N15—C15—C16 | 107.7 (6) | Ni1—N1—HB1 | 110.2 |
N15—C15—H15A | 110.2 | C1—N1—HA1 | 110.2 |
C16—C15—H15A | 110.2 | Ni1—N1—HA1 | 110.2 |
N15—C15—H15B | 110.2 | HB1—N1—HA1 | 108.5 |
C16—C15—H15B | 110.2 | C2—N2—Ni1 | 107.9 (5) |
H15A—C15—H15B | 108.5 | C2—N2—HB2 | 110.1 |
N16—C16—C15 | 108.5 (7) | Ni1—N2—HB2 | 110.1 |
N16—C16—H16A | 110.0 | C2—N2—HA2 | 110.1 |
C15—C16—H16A | 110.0 | Ni1—N2—HA2 | 110.1 |
N16—C16—H16B | 110.0 | HB2—N2—HA2 | 108.4 |
C15—C16—H16B | 110.0 | C6—N6—Ni1 | 108.4 (4) |
H16A—C16—H16B | 108.4 | C6—N6—HA6 | 110.0 |
N17—C17—C18 | 109.1 (7) | Ni1—N6—HA6 | 110.0 |
N17—C17—H17A | 109.9 | C6—N6—HB6 | 110.0 |
C18—C17—H17A | 109.9 | Ni1—N6—HB6 | 110.0 |
N17—C17—H17B | 109.9 | HA6—N6—HB6 | 108.4 |
C18—C17—H17B | 109.9 | C5—N5—Ni1 | 107.2 (4) |
H17A—C17—H17B | 108.3 | C5—N5—HB5 | 110.3 |
N18—C18—C17 | 108.9 (6) | Ni1—N5—HB5 | 110.3 |
N18—C18—H18A | 109.9 | C5—N5—HA5 | 110.3 |
C17—C18—H18A | 109.9 | Ni1—N5—HA5 | 110.3 |
N18—C18—H18B | 109.9 | HB5—N5—HA5 | 108.5 |
C17—C18—H18B | 109.9 | ||
N13—C13—C14—N14 | 56.1 (7) | N10—Ni2—N9—C9 | −12.8 (5) |
N3—C3—C4—N4 | 56.2 (11) | N8—Ni2—N9—C9 | 50 (3) |
N11—C11—C12—N12 | −56.2 (7) | N11—Ni2—N9—C9 | 172.6 (5) |
N7—C7—C8—N8 | −58.1 (10) | N7—Ni2—N9—C9 | 79.4 (5) |
N9—C9—C10—N10 | −56.3 (10) | C9—C10—N10—Ni2 | 42.7 (9) |
N15—C15—C16—N16 | 57.9 (10) | N12—Ni2—N10—C10 | 77.7 (5) |
N17—C17—C18—N18 | 55.5 (10) | N8—Ni2—N10—C10 | 169.3 (5) |
N1—C1—C2—N2 | 59.3 (10) | N11—Ni2—N10—C10 | 20 (2) |
N5—C5—C6—N6 | 55.6 (8) | N9—Ni2—N10—C10 | −16.1 (5) |
C14—C13—N13—Ni3 | −42.4 (6) | N7—Ni2—N10—C10 | −109.4 (5) |
N18—Ni3—N13—C13 | −171.2 (5) | C16—C15—N15—Ni3 | −44.0 (8) |
N16—Ni3—N13—C13 | −77.6 (5) | N18—Ni3—N15—C15 | 109.7 (5) |
N15—Ni3—N13—C13 | −27 (2) | N13—Ni3—N15—C15 | −35 (2) |
N14—Ni3—N13—C13 | 15.1 (5) | N16—Ni3—N15—C15 | 16.9 (5) |
N17—Ni3—N13—C13 | 106.1 (5) | N14—Ni3—N15—C15 | −76.0 (5) |
C13—C14—N14—Ni3 | −40.2 (7) | N17—Ni3—N15—C15 | −167.5 (5) |
N18—Ni3—N14—C14 | −35 (2) | C15—C16—N16—Ni3 | −41.7 (9) |
N13—Ni3—N14—C14 | 14.0 (5) | N18—Ni3—N16—C16 | −80.1 (6) |
N16—Ni3—N14—C14 | 107.0 (5) | N13—Ni3—N16—C16 | −173.2 (6) |
N15—Ni3—N14—C14 | −171.6 (5) | N15—Ni3—N16—C16 | 13.4 (6) |
N17—Ni3—N14—C14 | −79.3 (5) | N14—Ni3—N16—C16 | 105.0 (6) |
C4—C3—N3—Ni1 | −39.2 (8) | N17—Ni3—N16—C16 | −21 (3) |
N5—Ni1—N3—C3 | 104.6 (5) | C18—C17—N17—Ni3 | −38.3 (8) |
N4—Ni1—N3—C3 | 12.5 (5) | N18—Ni3—N17—C17 | 11.9 (5) |
N1—Ni1—N3—C3 | −81.3 (5) | N13—Ni3—N17—C17 | 104.4 (5) |
N2—Ni1—N3—C3 | −42 (2) | N16—Ni3—N17—C17 | −47 (3) |
N6—Ni1—N3—C3 | −173.4 (5) | N15—Ni3—N17—C17 | −81.8 (5) |
C3—C4—N4—Ni1 | −42.3 (9) | N14—Ni3—N17—C17 | −173.9 (5) |
N5—Ni1—N4—C4 | −77.3 (5) | C17—C18—N18—Ni3 | −43.0 (9) |
N1—Ni1—N4—C4 | 108.8 (5) | N13—Ni3—N18—C18 | −76.0 (6) |
N2—Ni1—N4—C4 | −169.8 (5) | N16—Ni3—N18—C18 | −169.6 (6) |
N3—Ni1—N4—C4 | 16.3 (5) | N15—Ni3—N18—C18 | 108.9 (6) |
N6—Ni1—N4—C4 | −23 (2) | N14—Ni3—N18—C18 | −27 (2) |
C12—C11—N11—Ni2 | 41.3 (7) | N17—Ni3—N18—C18 | 17.2 (6) |
N12—Ni2—N11—C11 | −14.9 (5) | C2—C1—N1—Ni1 | −44.4 (9) |
N10—Ni2—N11—C11 | 43.7 (19) | N5—Ni1—N1—C1 | −29 (2) |
N8—Ni2—N11—C11 | −105.8 (5) | N4—Ni1—N1—C1 | 109.6 (6) |
N9—Ni2—N11—C11 | 79.4 (5) | N2—Ni1—N1—C1 | 16.8 (5) |
N7—Ni2—N11—C11 | 172.9 (5) | N3—Ni1—N1—C1 | −167.9 (5) |
C11—C12—N12—Ni2 | 41.4 (7) | N6—Ni1—N1—C1 | −77.4 (6) |
N10—Ni2—N12—C12 | 173.7 (5) | C1—C2—N2—Ni1 | −42.7 (8) |
N8—Ni2—N12—C12 | 79.0 (5) | N5—Ni1—N2—C2 | −172.1 (5) |
N11—Ni2—N12—C12 | −14.2 (5) | N4—Ni1—N2—C2 | −79.3 (5) |
N9—Ni2—N12—C12 | −103.6 (5) | N1—Ni1—N2—C2 | 14.4 (5) |
N7—Ni2—N12—C12 | 44.2 (18) | N3—Ni1—N2—C2 | −25 (2) |
C8—C7—N7—Ni2 | 44.8 (8) | N6—Ni1—N2—C2 | 105.8 (5) |
N12—Ni2—N7—C7 | 17.9 (19) | C5—C6—N6—Ni1 | −38.2 (7) |
N10—Ni2—N7—C7 | −111.6 (5) | N5—Ni1—N6—C6 | 12.2 (5) |
N8—Ni2—N7—C7 | −17.4 (5) | N4—Ni1—N6—C6 | −43 (2) |
N11—Ni2—N7—C7 | 75.5 (5) | N1—Ni1—N6—C6 | −174.7 (5) |
N9—Ni2—N7—C7 | 165.7 (5) | N2—Ni1—N6—C6 | 103.9 (5) |
C7—C8—N8—Ni2 | 41.0 (8) | N3—Ni1—N6—C6 | −81.7 (5) |
N12—Ni2—N8—C8 | 171.8 (6) | C6—C5—N5—Ni1 | −43.1 (7) |
N10—Ni2—N8—C8 | 78.5 (6) | N4—Ni1—N5—C5 | −170.8 (5) |
N11—Ni2—N8—C8 | −106.2 (6) | N1—Ni1—N5—C5 | −32.3 (19) |
N9—Ni2—N8—C8 | 17 (3) | N2—Ni1—N5—C5 | −77.3 (5) |
N7—Ni2—N8—C8 | −13.5 (5) | N3—Ni1—N5—C5 | 106.8 (5) |
C10—C9—N9—Ni2 | 39.5 (8) | N6—Ni1—N5—C5 | 16.9 (5) |
N12—Ni2—N9—C9 | −105.5 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2E···O1 | 0.85 (4) | 1.97 (2) | 2.815 (9) | 179 (5) |
O2—H2F···Cl2 | 0.85 (4) | 2.45 (2) | 3.236 (8) | 155 (3) |
O4—H4E···Cl3 | 0.85 (4) | 2.64 (4) | 3.163 (8) | 121 (4) |
O5—H5E···Cl6 | 0.85 (4) | 2.56 (2) | 3.231 (9) | 136 (3) |
O5—H5F···O6 | 0.85 (4) | 2.17 (2) | 2.749 (4) | 125 (4) |
N3—HB3···O2 | 0.90 | 2.23 | 3.086 (5) | 158 |
N5—HA5···O2 | 0.90 | 2.21 | 3.064 (4) | 158 |
N6—HA6···Cl4 | 0.90 | 2.65 | 3.443 (3) | 147 |
N13—HA13···Cl4 | 0.90 | 2.64 | 3.440 (6) | 149 |
N13—HB13···Cl6 | 0.90 | 2.54 | 3.401 (5) | 160 |
N17—HB17···Cl6 | 0.90 | 2.50 | 3.371 (4) | 161 |