Towards the chemical control of molecular packing: syntheses and crystal structures of three trans-[NiL₄(NCS)₂] complexes

Three nickel(II) isothiocyanato complexes of the formula trans-[NiL₄(NCS)₂] (L = ethylisonicotinate, methylisonicotinate and 4-benzoylpyridine) have been prepared: [Ni(ethyl­isonicotinate)₄(NCS)₂] (I), [Ni(methylisonicotinate)₄(NCS)₂] (II) and [Ni(4-benzoylpyridine)₄(NCS)₂] (III). All three complexes are monomeric and have a distorted octahedral geometry around Ni^II. Despite their apparent molecular similarity, the crystal density of (III) (1.454 g cm^-3) is significantly higher than that of (I) and (II) (both 1.408 g cm^-3), suggesting that the molecular packing is most efficient in (III). A study of the molecular Hirshfeld surfaces, together with density functional theory (DFT) calculations, provide insights into the origin of the molecular packing features, and it is suggested that the greater crystal density of (III) results from smaller intermolecular electrostatic repulsions.

Computing details

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.

Figures

(I)

Crystal data

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) Å^3	0.45 × 0.14 × 0.12 mm
Z = 4

Data collection

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

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.030	H-atom parameters constrained
wR(F^2) = 0.072	w = 1/[σ^2(Fo^2) + (0.0288P)^2 + 1.7597P] where P = (Fo^2 + 2Fc^2)/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)

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

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)

(II)

Crystal data

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) Å^3	0.57 × 0.19 × 0.15 mm
Z = 10

Data collection

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

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.050	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.127	H-atom parameters constrained
S = 1.07	w = 1/[σ^2(Fo^2) + (0.063P)^2 + 5.5441P] where P = (Fo^2 + 2Fc^2)/3
14949 reflections	(Δ/σ)max = 0.001
1078 parameters	Δρmax = 1.00 e Å^−3
0 restraints	Δρmin = −0.55 e Å^−3

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

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—N13^i	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—N15^i	2.127 (3)	C49—C52	1.499 (5)
Ni3—N14	2.207 (3)	C50—C51	1.377 (5)
Ni3—N14^i	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
N13^i—Ni3—N13	180.00 (6)	C49—C50—H50	120.6
N13^i—Ni3—N15	89.65 (11)	N11—C51—C50	122.5 (3)
N13—Ni3—N15	90.35 (11)	N11—C51—H51	118.7
N13^i—Ni3—N15^i	90.35 (11)	C50—C51—H51	118.7
N13—Ni3—N15^i	89.65 (11)	O13—C52—O14	124.8 (3)
N15—Ni3—N15^i	180.0	O13—C52—C49	123.0 (3)
N13^i—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
N15^i—Ni3—N14	93.77 (10)	H53A—C53—H53B	109.5
N13^i—Ni3—N14^i	90.53 (11)	O14—C53—H53C	109.5
N13—Ni3—N14^i	89.47 (11)	H53A—C53—H53C	109.5
N15—Ni3—N14^i	93.77 (10)	H53B—C53—H53C	109.5
N15^i—Ni3—N14^i	86.23 (10)	N12—C54—C55	122.4 (3)
N14—Ni3—N14^i	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)
N15^i—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)
N14^i—Ni3—N13—C61	164.0 (15)	C47—C48—C49—C50	−1.8 (5)
N13^i—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)
N15^i—Ni3—N14—C62	−110.4 (3)	C47—N11—C51—C50	−1.4 (5)
N13^i—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)
N15^i—Ni3—N14—C66	70.0 (3)	C53—O14—C52—C49	−175.2 (3)
N13^i—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)
N14^i—Ni3—N15—C69	47.3 (3)	C48—C49—C52—O14	−19.2 (5)
N13^i—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)
N14^i—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.

(III)

Crystal data

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) Å^3	0.23 × 0.21 × 0.20 mm
Z = 2

Data collection

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

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.027	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.072	H-atom parameters constrained
S = 0.88	w = 1/[σ^2(Fo^2) + (0.0395P)^2 + 1.5386P] where P = (Fo^2 + 2Fc^2)/3
6604 reflections	(Δ/σ)max = 0.002
286 parameters	Δρmax = 0.49 e Å^−3
0 restraints	Δρmin = −0.43 e Å^−3

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	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*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Geometric parameters (Å, º)

Ni1—N1^i	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—N3^i	2.1613 (8)	C11—H11	0.9500
Ni1—N2^i	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
N1^i—Ni1—N1	180.0	C9—C10—H10	119.9
N1^i—Ni1—N3	89.08 (3)	C11—C10—H10	119.9
N1—Ni1—N3	90.92 (3)	C12—C11—C10	120.16 (10)
N1^i—Ni1—N3^i	90.91 (3)	C12—C11—H11	119.9
N1—Ni1—N3^i	89.08 (3)	C10—C11—H11	119.9
N3—Ni1—N3^i	180.0	C11—C12—C13	119.90 (10)
N1^i—Ni1—N2^i	89.77 (3)	C11—C12—H12	120.0
N1—Ni1—N2^i	90.23 (3)	C13—C12—H12	120.0
N3—Ni1—N2^i	91.11 (3)	C12—C13—C8	120.19 (9)
N3^i—Ni1—N2^i	88.90 (3)	C12—C13—H13	119.9
N1^i—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
N3^i—Ni1—N2	91.10 (3)	C16—C15—H15	118.4
N2^i—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.