New homodinuclear tris­(3-alkyl­pyrazol­yl)borate complexes of Co^II and Ni^II with a tetra­acetyl­ethane dianion as a bridging ligand

Polynuclear complexes and coordination polymers of 3d metals have attracted significant inter­est evoked by a number of their unique properties. One of the most common approaches to the directed synthesis of coordination polymers is the linking of pre-prepared discrete coordination units by polydentate ligands. The formation of polynuclear complexes is usually a spontaneous process and precise prediction of the products of such reactions is virtually impossible in most cases. Tris(pyrazol­yl)borates (Tp) act as tripodal `capping' ligands which form stable complexes with 3d metal ions. In such 1:1 compounds, three metal-ion coordination sites are occupied by N atoms from a Tp anion. This limits the number of remaining coordination sites, and thus the number of additional ligands which may coordinate, and opens an attractive approach for the directed design of desirable structures by exploiting ligands with appropriate composition and topology. In the present study, Tp anions with neopentyl [Tp<sup>Np</sup>, tris­(3-neo­pentyl­pyrazol­yl)borate] and cyclo­hexyl [Tp<sup>Cy</sup>, tris­(3-cyclo­hexyl­pyrazol­yl)borate] substituents were used as `capping' ligands and the dianion of tetra­acetyl­ethane (3,4-di­acetyl­hexa-2,4-diene-2,5-diolate, tae²⁻) was employed as a bridge. The dinuclear complexes (μ-3,4-di­acetyl­hexa-2,4-diene-2,5-diolato-κ⁴O²,O³:O⁴,O⁵)bis­{[tris­(3-cyclo­hexyl-1H-pyrazol-1-yl-κN²)borato]cobalt(II)} aceto­nitrile disolvate, [Co₂(C₂₇H₄₀BN₆)₂(C₁₀H₁₂O₄)]·2CH₃CN, (I)·2CH₃CN, and (μ-3,4-di­acetyl­hexa-2,4-diene-2,5-diolato-κ⁴O²,O³:O⁴,O⁵)bis­{[tris­(3-neo­pentyl-1H-pyrazol-1-yl-κN²)borato]nickel(II)}, [Ni₂(C₂₄H₄₀BN₆)₂(C₁₀H₁₂O₄)], (II), were synthesized by the reaction of the mononuclear complexes Tp^CyCoCl or Tp^NpNiCl with H₂tae (3,4-di­acetyl­hexane-2,5-dione or tetra­acetyl­ethane) in the presence of NEt₃ as base. Compounds (I) and (II) were characterized by mass spectrometry, elemental analysis, and X-ray crystallography. They possess similar mol­ecular structures, X-ray diffraction revealing them to be dinuclear in nature and composed of discrete Tp–M units in which two metal ions are linked by a tae²⁻ dianion. Each metal ion possesses a five-coordinate square-pyramidal environment. The inter­planar angles between the acetyl­acetonate fragments are significantly smaller than the near-90° values commonly observed.

Computing details

For both compounds, data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2013); data reduction: SAINT (Bruker, 2013); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015) and SHELXLE (Hübschle et al., 2011); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015).

(Ix2CH3CN) (µ-3,4-Diacetylhexa-2,4-diene-2,5-diolato-κ⁴O²,O³:O⁴,O⁵)bis{[tris(3-cyclohexyl-1H-pyrazol-1-yl-κN²)borato]cobalt(II)} acetonitrile disolvate

Crystal data

[Co2(C27H40BN6)2(C10H12O4)]·2C2H3N	Z = 2
Mr = 1315.08	F(000) = 1400
Triclinic, P1	Dx = 1.287 Mg m^−3
a = 13.175 (7) Å	Mo Kα radiation, λ = 0.71073 Å
b = 13.672 (7) Å	Cell parameters from 656 reflections
c = 19.571 (10) Å	θ = 3.3–28.1°
α = 77.203 (7)°	µ = 0.55 mm^−1
β = 80.890 (7)°	T = 100 K
γ = 89.522 (7)°	Needle, red
V = 3393 (3) Å^3	0.55 × 0.11 × 0.10 mm

Data collection

Bruker SMART APEX CCD diffractometer	16151 independent reflections
Radiation source: fine-focus sealed tube	9221 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.123
ω scans	θmax = 28.3°, θmin = 1.1°
Absorption correction: multi-scan (TWINABS; Sheldrick, 2007)	h = −17→17
Tmin = 0.728, Tmax = 0.862	k = −17→18
35732 measured reflections	l = 0→25

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)] = 0.083	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.229	H-atom parameters constrained
S = 1.17	w = 1/[σ^2(Fo^2) + 15.1876P] where P = (Fo^2 + 2Fc^2)/3
16151 reflections	(Δ/σ)max < 0.001
829 parameters	Δρmax = 0.88 e Å^−3
3 restraints	Δρmin = −1.06 e Å^−3

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. The small crystals were found to be only weakly diffracting and data were collected with an exposure time of 2 minutes per frame. The crystal under investigation was found to be non-merohedrically twinned. The orientation matrices for the two components were identified using the program Cell_Now, with the two components being related by a 180 degree rotation around the reciprocal axis (1 -1 0). The two components were integrated using Saint, resulting in a total of 51292 reflections. 15560 reflections (8864 unique) involved component 1 only (mean I/σ = 3.4), 15560 reflections (8866 unique) involved component 2 only (mean I/σ = 3.3), and 20172 reflections (11715 unique) involved both components (mean I/σ = 3.8). The exact twin matrix identified by the integration program was found to be 0.02517 -0.97472 0.04145, -1.02527 -0.02514 -0.04155, -0.00005 0.00025 -1.00003.

The data were corrected for absorption using twinabs, and the structure was solved using direct methods with only the non-overlapping reflections of component 1. The structure was refined using the hklf 5 routine with all reflections of component 1 (including the overlapping ones) with a resolution better than 0.75 Angstrom, resulting in a BASF value of 0.503 (2).

The Rint value (_diffrn_reflns_av_R_equivalents) and the total number of reflections (_diffrn_reflns_number) are given for all reflections before the cutoff at 0.75 Angstrom and is based on agreement between observed single and composite intensities and those calculated from refined unique intensities and twin fractions (TWINABS (Sheldrick, 2007)).

One of the interstitial acetonitrile molecules is disordered over two mutually exclusive sites with a refined occupancy ratio of 0.81 (1) to 0.19 (1). The two moieties were refined to have similar geometries, equivalent atoms were constrained to have identical ADPs.

Reflection 1 0 0 was affected by the beam stop and was omitted from the refinement.

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
B1	0.4097 (7)	0.8258 (7)	0.2867 (5)	0.0206 (19)
H1A	0.4562	0.8785	0.2942	0.025*
B2	−0.3107 (7)	0.0845 (7)	0.2102 (5)	0.023 (2)
H2A	−0.3618	0.0377	0.2006	0.027*
C1	0.4320 (6)	0.7218 (6)	0.4128 (4)	0.0233 (18)
H1	0.4718	0.7691	0.4270	0.028*
C2	0.3988 (6)	0.6279 (6)	0.4530 (4)	0.0252 (19)
H2	0.4118	0.5981	0.4994	0.030*
C3	0.3421 (6)	0.5857 (6)	0.4116 (4)	0.0180 (17)
C4	0.2868 (6)	0.4867 (6)	0.4269 (4)	0.0189 (16)
H4	0.2753	0.4731	0.3806	0.023*
C5	0.3505 (6)	0.4014 (6)	0.4617 (4)	0.0238 (17)
H5A	0.4169	0.3996	0.4303	0.029*
H5B	0.3654	0.4140	0.5071	0.029*
C6	0.2940 (6)	0.3005 (6)	0.4758 (5)	0.0279 (18)
H6A	0.3345	0.2478	0.5018	0.033*
H6B	0.2875	0.2837	0.4300	0.033*
C7	0.1871 (7)	0.3017 (6)	0.5191 (4)	0.0298 (19)
H7A	0.1504	0.2371	0.5235	0.036*
H7B	0.1939	0.3086	0.5675	0.036*
C8	0.1245 (6)	0.3871 (6)	0.4851 (4)	0.0230 (17)
H8A	0.0580	0.3885	0.5164	0.028*
H8B	0.1100	0.3755	0.4394	0.028*
C9	0.1818 (6)	0.4885 (6)	0.4721 (4)	0.0200 (16)
H9A	0.1409	0.5423	0.4477	0.024*
H9B	0.1905	0.5032	0.5182	0.024*
C10	0.2674 (7)	0.9601 (6)	0.2764 (4)	0.0257 (18)
H10	0.3044	1.0141	0.2852	0.031*
C11	0.1697 (6)	0.9646 (6)	0.2607 (4)	0.0241 (18)
H11	0.1266	1.0209	0.2557	0.029*
C12	0.1470 (6)	0.8673 (5)	0.2535 (4)	0.0179 (16)
C13	0.0516 (6)	0.8263 (6)	0.2366 (4)	0.0213 (16)
H13	0.0631	0.7544	0.2350	0.026*
C14	−0.0406 (6)	0.8296 (6)	0.2938 (4)	0.0259 (18)
H14A	−0.0265	0.7901	0.3400	0.031*
H14B	−0.0517	0.8999	0.2981	0.031*
C15	−0.1369 (6)	0.7876 (7)	0.2759 (4)	0.0291 (19)
H15A	−0.1964	0.7937	0.3125	0.035*
H15B	−0.1284	0.7154	0.2763	0.035*
C16	−0.1580 (6)	0.8434 (6)	0.2031 (4)	0.0257 (18)
H16A	−0.2193	0.8127	0.1917	0.031*
H16B	−0.1728	0.9142	0.2040	0.031*
C17	−0.0671 (6)	0.8395 (6)	0.1463 (4)	0.0276 (18)
H17A	−0.0814	0.8789	0.1001	0.033*
H17B	−0.0565	0.7692	0.1421	0.033*
C18	0.0302 (6)	0.8815 (7)	0.1636 (4)	0.0259 (18)
H18A	0.0223	0.9538	0.1628	0.031*
H18B	0.0893	0.8746	0.1270	0.031*
C19	0.5321 (6)	0.8299 (6)	0.1672 (4)	0.0213 (17)
H19	0.5816	0.8782	0.1704	0.026*
C20	0.5300 (6)	0.7864 (6)	0.1099 (4)	0.0221 (18)
H20	0.5775	0.7977	0.0669	0.026*
C21	0.4433 (6)	0.7225 (6)	0.1288 (4)	0.0159 (16)
C22	0.3963 (6)	0.6620 (6)	0.0866 (4)	0.0178 (16)
H22	0.3866	0.5915	0.1152	0.021*
C23	0.4632 (6)	0.6600 (6)	0.0161 (4)	0.0234 (17)
H23A	0.5303	0.6310	0.0249	0.028*
H23B	0.4762	0.7293	−0.0125	0.028*
C24	0.4113 (7)	0.5978 (7)	−0.0251 (4)	0.0280 (19)
H24A	0.4561	0.5984	−0.0708	0.034*
H24B	0.4027	0.5275	0.0023	0.034*
C25	0.3076 (7)	0.6375 (7)	−0.0392 (5)	0.031 (2)
H25A	0.2748	0.5936	−0.0639	0.037*
H25B	0.3162	0.7058	−0.0701	0.037*
C26	0.2391 (6)	0.6407 (6)	0.0313 (4)	0.0239 (18)
H26A	0.1727	0.6706	0.0217	0.029*
H26B	0.2248	0.5715	0.0599	0.029*
C27	0.2897 (6)	0.7015 (6)	0.0732 (4)	0.0231 (18)
H27A	0.2450	0.6990	0.1193	0.028*
H27B	0.2971	0.7724	0.0468	0.028*
C28	0.2644 (6)	0.3901 (6)	0.1863 (4)	0.0220 (17)
H28A	0.3236	0.4204	0.1513	0.033*
H28B	0.2111	0.3706	0.1618	0.033*
H28C	0.2860	0.3306	0.2182	0.033*
C29	0.2223 (6)	0.4646 (5)	0.2286 (4)	0.0191 (16)
C30	0.1180 (5)	0.4585 (5)	0.2616 (4)	0.0176 (16)
C31	0.0787 (6)	0.5266 (5)	0.3033 (4)	0.0172 (16)
C32	−0.0289 (6)	0.5114 (6)	0.3447 (4)	0.0226 (17)
H32A	−0.0426	0.5633	0.3721	0.034*
H32B	−0.0356	0.4451	0.3772	0.034*
H32C	−0.0785	0.5158	0.3118	0.034*
C33	−0.0160 (6)	0.5253 (5)	0.1589 (4)	0.0197 (16)
H33A	−0.0569	0.5319	0.1205	0.030*
H33B	0.0563	0.5421	0.1386	0.030*
H33C	−0.0413	0.5712	0.1894	0.030*
C34	−0.0255 (6)	0.4179 (5)	0.2025 (4)	0.0158 (15)
C35	0.0449 (5)	0.3829 (5)	0.2494 (4)	0.0153 (15)
C36	0.0456 (6)	0.2815 (5)	0.2825 (4)	0.0161 (15)
C37	0.1248 (6)	0.2423 (6)	0.3292 (4)	0.0218 (17)
H37A	0.0899	0.2077	0.3763	0.033*
H37B	0.1670	0.2985	0.3338	0.033*
H37C	0.1688	0.1953	0.3078	0.033*
C38	−0.3157 (7)	−0.0357 (6)	0.3361 (4)	0.0245 (19)
H38	−0.3627	−0.0856	0.3320	0.029*
C39	−0.2773 (6)	−0.0309 (6)	0.3961 (4)	0.0243 (18)
H39	−0.2916	−0.0758	0.4413	0.029*
C40	−0.2128 (6)	0.0540 (6)	0.3769 (4)	0.0219 (18)
C41	−0.1549 (6)	0.1006 (6)	0.4230 (4)	0.0220 (18)
H41	−0.0809	0.1085	0.4006	0.026*
C42	−0.1611 (7)	0.0354 (7)	0.4982 (4)	0.030 (2)
H42A	−0.2338	0.0255	0.5214	0.036*
H42B	−0.1326	−0.0312	0.4958	0.036*
C43	−0.1006 (8)	0.0859 (8)	0.5416 (5)	0.041 (2)
H43A	−0.1046	0.0430	0.5900	0.049*
H43B	−0.0274	0.0933	0.5193	0.049*
C44	−0.1414 (7)	0.1873 (8)	0.5467 (5)	0.035 (2)
H44A	−0.1001	0.2187	0.5746	0.042*
H44B	−0.2134	0.1800	0.5715	0.042*
C45	−0.1368 (8)	0.2547 (7)	0.4723 (5)	0.034 (2)
H45A	−0.1677	0.3200	0.4761	0.041*
H45B	−0.0642	0.2676	0.4493	0.041*
C46	−0.1949 (7)	0.2045 (6)	0.4272 (4)	0.0249 (19)
H46A	−0.2688	0.1985	0.4477	0.030*
H46B	−0.1880	0.2473	0.3787	0.030*
C47	−0.4557 (6)	0.2165 (6)	0.2096 (4)	0.0227 (17)
H47	−0.5092	0.1792	0.1988	0.027*
C48	−0.4624 (6)	0.3116 (6)	0.2223 (5)	0.0272 (19)
H48	−0.5208	0.3528	0.2217	0.033*
C49	−0.3672 (6)	0.3347 (6)	0.2362 (4)	0.0186 (16)
C50	−0.3328 (6)	0.4279 (6)	0.2544 (4)	0.0211 (16)
H50	−0.2596	0.4196	0.2618	0.025*
C51	−0.3956 (7)	0.4420 (6)	0.3240 (4)	0.0268 (18)
H51A	−0.4694	0.4454	0.3194	0.032*
H51B	−0.3871	0.3833	0.3625	0.032*
C52	−0.3623 (7)	0.5371 (6)	0.3437 (5)	0.031 (2)
H52A	−0.4071	0.5459	0.3874	0.037*
H52B	−0.2908	0.5309	0.3533	0.037*
C53	−0.3689 (7)	0.6280 (6)	0.2842 (4)	0.0290 (19)
H53A	−0.4414	0.6377	0.2772	0.035*
H53B	−0.3442	0.6886	0.2971	0.035*
C54	−0.3044 (7)	0.6145 (6)	0.2159 (4)	0.031 (2)
H54A	−0.2312	0.6104	0.2219	0.037*
H54B	−0.3114	0.6736	0.1774	0.037*
C55	−0.3367 (7)	0.5206 (6)	0.1951 (4)	0.0272 (19)
H55A	−0.2905	0.5122	0.1518	0.033*
H55B	−0.4075	0.5277	0.1841	0.033*
C56	−0.2010 (6)	0.0749 (6)	0.0887 (4)	0.0212 (17)
H56	−0.2476	0.0361	0.0724	0.025*
C57	−0.1077 (6)	0.1114 (6)	0.0526 (4)	0.0220 (18)
H57	−0.0760	0.1023	0.0074	0.026*
C58	−0.0677 (6)	0.1653 (6)	0.0959 (4)	0.0194 (17)
C59	0.0302 (6)	0.2245 (5)	0.0842 (4)	0.0172 (15)
H59	0.0399	0.2395	0.1306	0.021*
C60	0.1233 (6)	0.1681 (6)	0.0584 (4)	0.0255 (18)
H60A	0.1280	0.1048	0.0939	0.031*
H60B	0.1138	0.1504	0.0134	0.031*
C61	0.2232 (6)	0.2289 (6)	0.0466 (5)	0.0296 (19)
H61A	0.2807	0.1908	0.0272	0.036*
H61B	0.2370	0.2404	0.0925	0.036*
C62	0.2169 (6)	0.3303 (6)	−0.0053 (4)	0.0290 (19)
H62A	0.2800	0.3711	−0.0089	0.035*
H62B	0.2127	0.3189	−0.0530	0.035*
C63	0.1239 (6)	0.3870 (6)	0.0191 (4)	0.0245 (18)
H63A	0.1323	0.4055	0.0640	0.029*
H63B	0.1195	0.4497	−0.0169	0.029*
C64	0.0255 (6)	0.3260 (6)	0.0303 (4)	0.0241 (18)
H64A	0.0135	0.3130	−0.0156	0.029*
H64B	−0.0328	0.3645	0.0482	0.029*
C65	0.4350 (9)	1.0318 (7)	0.0803 (5)	0.040 (3)
C66	0.3423 (8)	0.9714 (7)	0.0861 (6)	0.042 (2)
H66A	0.3418	0.9497	0.0416	0.063*
H66B	0.2817	1.0114	0.0953	0.063*
H66C	0.3409	0.9123	0.1252	0.063*
Co1	0.26640 (8)	0.65827 (7)	0.26388 (5)	0.0161 (2)
Co2	−0.14836 (8)	0.22898 (7)	0.23995 (5)	0.0164 (2)
N1	0.3419 (5)	0.6518 (5)	0.3491 (3)	0.0156 (13)
N2	0.3982 (5)	0.7348 (5)	0.3498 (3)	0.0185 (14)
N3	0.2278 (5)	0.8082 (5)	0.2655 (3)	0.0196 (14)
N4	0.3026 (5)	0.8678 (5)	0.2774 (3)	0.0184 (13)
N5	0.3973 (5)	0.7256 (5)	0.1948 (3)	0.0184 (14)
N6	0.4514 (5)	0.7919 (5)	0.2178 (3)	0.0151 (13)
N7	−0.2122 (5)	0.0974 (5)	0.3096 (3)	0.0193 (14)
N8	−0.2760 (5)	0.0420 (5)	0.2837 (3)	0.0202 (15)
N9	−0.3038 (5)	0.2601 (5)	0.2299 (3)	0.0186 (14)
N10	−0.3591 (5)	0.1861 (5)	0.2152 (3)	0.0206 (14)
N11	−0.1359 (5)	0.1593 (5)	0.1561 (3)	0.0181 (14)
N12	−0.2169 (5)	0.1024 (5)	0.1514 (4)	0.0207 (15)
N13	0.5090 (9)	1.0766 (7)	0.0763 (5)	0.064 (3)
O1	0.2891 (4)	0.5284 (4)	0.2349 (2)	0.0156 (11)
O2	0.1273 (4)	0.6025 (4)	0.3106 (3)	0.0191 (11)
O3	−0.0153 (4)	0.2127 (4)	0.2760 (3)	0.0204 (12)
O4	−0.0992 (4)	0.3681 (4)	0.1917 (3)	0.0188 (11)
N14	0.4296 (9)	−0.0188 (10)	0.4253 (6)	0.060 (3)	0.808 (10)
C67	0.4710 (9)	0.0572 (10)	0.4137 (6)	0.038 (3)	0.808 (10)
C68	0.525 (2)	0.156 (3)	0.3997 (14)	0.037 (5)	0.808 (10)
H68A	0.5322	0.1733	0.4449	0.056*	0.808 (10)
H68B	0.4854	0.2079	0.3729	0.056*	0.808 (10)
H68C	0.5935	0.1536	0.3720	0.056*	0.808 (10)
N14B	0.362 (3)	0.108 (4)	0.365 (2)	0.060 (3)	0.192 (10)
C67B	0.437 (3)	0.128 (4)	0.383 (2)	0.038 (3)	0.192 (10)
C68B	0.529 (9)	0.147 (13)	0.414 (8)	0.037 (5)	0.192 (10)
H68D	0.5206	0.2098	0.4303	0.056*	0.192 (10)
H68E	0.5901	0.1524	0.3777	0.056*	0.192 (10)
H68F	0.5357	0.0915	0.4541	0.056*	0.192 (10)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
B1	0.022 (4)	0.020 (4)	0.020 (5)	−0.007 (4)	0.000 (4)	−0.005 (4)
B2	0.025 (5)	0.023 (5)	0.021 (5)	−0.012 (4)	−0.003 (4)	−0.006 (4)
C1	0.027 (4)	0.021 (4)	0.024 (4)	−0.005 (3)	−0.008 (4)	−0.007 (3)
C2	0.029 (4)	0.032 (5)	0.018 (4)	0.000 (4)	−0.008 (4)	−0.010 (4)
C3	0.017 (4)	0.022 (4)	0.013 (4)	0.001 (3)	0.003 (3)	−0.004 (3)
C4	0.023 (4)	0.020 (4)	0.014 (4)	−0.001 (3)	−0.002 (3)	−0.004 (3)
C5	0.025 (4)	0.024 (4)	0.021 (4)	0.001 (3)	−0.005 (3)	−0.002 (3)
C6	0.028 (4)	0.022 (4)	0.032 (5)	−0.001 (3)	−0.004 (4)	−0.002 (4)
C7	0.034 (5)	0.023 (4)	0.026 (5)	−0.010 (4)	0.001 (4)	0.006 (3)
C8	0.025 (4)	0.026 (4)	0.017 (4)	−0.006 (3)	0.004 (3)	−0.006 (3)
C9	0.021 (4)	0.026 (4)	0.013 (4)	−0.006 (3)	−0.001 (3)	−0.008 (3)
C10	0.038 (5)	0.013 (4)	0.029 (5)	−0.002 (3)	−0.013 (4)	−0.006 (3)
C11	0.030 (4)	0.017 (4)	0.027 (4)	−0.001 (3)	−0.006 (4)	−0.007 (3)
C12	0.027 (4)	0.016 (4)	0.006 (3)	−0.002 (3)	0.006 (3)	0.003 (3)
C13	0.025 (4)	0.016 (4)	0.026 (4)	0.000 (3)	−0.008 (4)	−0.008 (3)
C14	0.026 (4)	0.031 (5)	0.018 (4)	−0.001 (4)	−0.003 (4)	−0.001 (4)
C15	0.020 (4)	0.034 (5)	0.029 (5)	−0.003 (4)	−0.002 (4)	0.002 (4)
C16	0.027 (4)	0.025 (4)	0.024 (4)	0.005 (3)	−0.007 (3)	−0.001 (3)
C17	0.037 (5)	0.027 (4)	0.021 (4)	0.006 (4)	−0.013 (4)	−0.007 (3)
C18	0.022 (4)	0.032 (4)	0.023 (4)	−0.001 (3)	0.001 (3)	−0.006 (4)
C19	0.015 (4)	0.020 (4)	0.026 (4)	−0.003 (3)	0.004 (3)	−0.005 (3)
C20	0.022 (4)	0.027 (4)	0.014 (4)	−0.007 (3)	0.002 (3)	−0.003 (3)
C21	0.014 (4)	0.020 (4)	0.011 (4)	−0.002 (3)	0.001 (3)	−0.001 (3)
C22	0.023 (4)	0.018 (4)	0.014 (4)	0.002 (3)	−0.002 (3)	−0.006 (3)
C23	0.021 (4)	0.022 (4)	0.025 (4)	−0.001 (3)	0.002 (3)	−0.004 (3)
C24	0.038 (5)	0.033 (5)	0.017 (4)	0.005 (4)	−0.001 (4)	−0.018 (4)
C25	0.033 (5)	0.034 (5)	0.029 (5)	0.002 (4)	−0.009 (4)	−0.011 (4)
C26	0.025 (4)	0.029 (4)	0.020 (4)	−0.001 (4)	−0.008 (4)	−0.008 (4)
C27	0.021 (4)	0.031 (4)	0.019 (4)	0.004 (3)	−0.002 (3)	−0.010 (4)
C28	0.022 (4)	0.020 (4)	0.024 (4)	−0.002 (3)	−0.001 (3)	−0.007 (3)
C29	0.022 (4)	0.014 (4)	0.023 (4)	−0.002 (3)	−0.009 (3)	−0.004 (3)
C30	0.015 (4)	0.017 (4)	0.020 (4)	−0.007 (3)	−0.001 (3)	−0.004 (3)
C31	0.016 (4)	0.016 (4)	0.017 (4)	0.003 (3)	−0.001 (3)	0.001 (3)
C32	0.022 (4)	0.020 (4)	0.027 (4)	−0.004 (3)	−0.002 (4)	−0.009 (3)
C33	0.024 (4)	0.017 (4)	0.017 (4)	−0.004 (3)	−0.003 (3)	0.000 (3)
C34	0.016 (4)	0.017 (4)	0.015 (4)	−0.004 (3)	0.000 (3)	−0.006 (3)
C35	0.018 (4)	0.016 (3)	0.014 (4)	−0.002 (3)	−0.001 (3)	−0.007 (3)
C36	0.021 (4)	0.018 (4)	0.009 (4)	0.001 (3)	0.002 (3)	−0.004 (3)
C37	0.027 (4)	0.019 (4)	0.023 (4)	0.001 (3)	−0.011 (4)	−0.005 (3)
C38	0.026 (4)	0.022 (4)	0.022 (4)	−0.007 (3)	0.009 (4)	−0.008 (4)
C39	0.030 (4)	0.018 (4)	0.020 (4)	−0.003 (3)	0.005 (4)	−0.001 (3)
C40	0.025 (4)	0.021 (4)	0.019 (4)	0.003 (3)	0.000 (4)	−0.006 (3)
C41	0.022 (4)	0.020 (4)	0.018 (4)	−0.002 (3)	0.004 (3)	0.003 (3)
C42	0.036 (5)	0.036 (5)	0.017 (4)	0.009 (4)	−0.005 (4)	−0.001 (4)
C43	0.042 (6)	0.053 (6)	0.027 (5)	0.006 (5)	−0.010 (4)	−0.006 (5)
C44	0.031 (5)	0.054 (6)	0.025 (5)	0.000 (4)	−0.002 (4)	−0.018 (4)
C45	0.043 (6)	0.038 (5)	0.026 (5)	0.003 (4)	−0.007 (4)	−0.016 (4)
C46	0.034 (5)	0.022 (4)	0.021 (4)	−0.002 (4)	−0.010 (4)	−0.007 (4)
C47	0.019 (4)	0.028 (4)	0.021 (4)	−0.003 (3)	−0.002 (3)	−0.004 (3)
C48	0.012 (4)	0.033 (5)	0.035 (5)	0.006 (3)	−0.001 (4)	−0.006 (4)
C49	0.019 (4)	0.023 (4)	0.013 (4)	−0.002 (3)	0.001 (3)	−0.005 (3)
C50	0.021 (4)	0.022 (4)	0.019 (4)	0.003 (3)	0.001 (3)	−0.003 (3)
C51	0.036 (5)	0.021 (4)	0.019 (4)	0.004 (3)	0.004 (4)	−0.002 (3)
C52	0.041 (5)	0.031 (5)	0.023 (4)	0.008 (4)	−0.004 (4)	−0.010 (4)
C53	0.031 (5)	0.022 (4)	0.038 (5)	0.008 (3)	−0.007 (4)	−0.014 (4)
C54	0.043 (5)	0.026 (4)	0.022 (4)	0.002 (4)	0.001 (4)	−0.008 (4)
C55	0.038 (5)	0.023 (4)	0.020 (4)	0.000 (4)	−0.001 (4)	−0.005 (3)
C56	0.031 (4)	0.019 (4)	0.016 (4)	−0.003 (3)	−0.006 (4)	−0.007 (3)
C57	0.026 (4)	0.028 (4)	0.012 (4)	0.000 (3)	0.001 (3)	−0.005 (3)
C58	0.030 (4)	0.018 (4)	0.012 (4)	0.002 (3)	−0.007 (3)	−0.003 (3)
C59	0.022 (4)	0.018 (4)	0.011 (4)	−0.001 (3)	0.000 (3)	−0.003 (3)
C60	0.026 (4)	0.028 (4)	0.023 (4)	0.009 (3)	−0.004 (3)	−0.007 (3)
C61	0.022 (4)	0.030 (5)	0.034 (5)	0.002 (4)	−0.004 (4)	−0.004 (4)
C62	0.029 (4)	0.033 (5)	0.022 (4)	−0.005 (4)	0.000 (4)	−0.001 (4)
C63	0.029 (4)	0.023 (4)	0.021 (4)	−0.006 (3)	−0.007 (4)	−0.001 (3)
C64	0.024 (4)	0.023 (4)	0.024 (4)	0.002 (3)	−0.005 (4)	−0.001 (3)
C65	0.079 (8)	0.022 (5)	0.024 (5)	0.005 (5)	−0.028 (5)	−0.002 (4)
C66	0.042 (6)	0.029 (5)	0.053 (6)	0.006 (4)	−0.015 (5)	0.000 (5)
Co1	0.0195 (5)	0.0159 (5)	0.0130 (5)	−0.0046 (4)	−0.0016 (4)	−0.0039 (4)
Co2	0.0185 (5)	0.0154 (5)	0.0152 (5)	−0.0037 (4)	−0.0010 (4)	−0.0042 (4)
N1	0.021 (3)	0.016 (3)	0.010 (3)	−0.008 (3)	0.003 (3)	−0.006 (3)
N2	0.018 (3)	0.021 (3)	0.019 (3)	0.000 (3)	−0.002 (3)	−0.011 (3)
N3	0.019 (3)	0.018 (3)	0.023 (3)	−0.005 (3)	−0.002 (3)	−0.006 (3)
N4	0.022 (3)	0.017 (3)	0.017 (3)	−0.001 (3)	0.000 (3)	−0.008 (3)
N5	0.022 (3)	0.014 (3)	0.021 (4)	−0.005 (3)	−0.004 (3)	−0.007 (3)
N6	0.017 (3)	0.016 (3)	0.011 (3)	−0.004 (2)	0.004 (3)	−0.003 (3)
N7	0.020 (3)	0.017 (3)	0.020 (4)	−0.002 (3)	0.000 (3)	−0.003 (3)
N8	0.026 (4)	0.022 (3)	0.011 (3)	−0.007 (3)	0.006 (3)	−0.007 (3)
N9	0.019 (3)	0.021 (3)	0.015 (3)	−0.003 (3)	0.002 (3)	−0.006 (3)
N10	0.013 (3)	0.026 (4)	0.024 (4)	−0.005 (3)	0.001 (3)	−0.011 (3)
N11	0.022 (3)	0.016 (3)	0.013 (3)	−0.003 (3)	0.000 (3)	0.002 (3)
N12	0.021 (3)	0.015 (3)	0.025 (4)	−0.004 (3)	0.001 (3)	−0.004 (3)
N13	0.096 (8)	0.032 (5)	0.070 (7)	−0.021 (5)	−0.048 (6)	0.005 (5)
O1	0.019 (3)	0.020 (3)	0.008 (2)	−0.004 (2)	0.002 (2)	−0.005 (2)
O2	0.022 (3)	0.016 (3)	0.021 (3)	−0.004 (2)	−0.002 (2)	−0.007 (2)
O3	0.022 (3)	0.016 (3)	0.023 (3)	−0.003 (2)	−0.005 (2)	−0.002 (2)
O4	0.019 (3)	0.015 (3)	0.022 (3)	−0.004 (2)	−0.006 (2)	−0.002 (2)
N14	0.051 (7)	0.072 (8)	0.054 (7)	−0.019 (6)	0.024 (6)	−0.030 (7)
C67	0.033 (6)	0.043 (7)	0.033 (7)	−0.006 (5)	0.005 (5)	−0.006 (6)
C68	0.034 (6)	0.043 (10)	0.032 (14)	0.004 (6)	0.004 (7)	−0.008 (10)
N14B	0.051 (7)	0.072 (8)	0.054 (7)	−0.019 (6)	0.024 (6)	−0.030 (7)
C67B	0.033 (6)	0.043 (7)	0.033 (7)	−0.006 (5)	0.005 (5)	−0.006 (6)
C68B	0.034 (6)	0.043 (10)	0.032 (14)	0.004 (6)	0.004 (7)	−0.008 (10)

Geometric parameters (Å, º)

B1—N2	1.535 (11)	C37—H37C	0.9800
B1—N6	1.540 (11)	C38—N8	1.346 (10)
B1—N4	1.541 (11)	C38—C39	1.365 (11)
B1—H1A	1.0000	C38—H38	0.9500
B2—N12	1.530 (11)	C39—C40	1.390 (11)
B2—N10	1.540 (11)	C39—H39	0.9500
B2—N8	1.564 (11)	C40—N7	1.316 (10)
B2—H2A	1.0000	C40—C41	1.512 (11)
C1—N2	1.350 (10)	C41—C46	1.525 (11)
C1—C2	1.383 (12)	C41—C42	1.533 (11)
C1—H1	0.9500	C41—H41	1.0000
C2—C3	1.398 (10)	C42—C43	1.522 (13)
C2—H2	0.9500	C42—H42A	0.9900
C3—N1	1.350 (10)	C42—H42B	0.9900
C3—C4	1.491 (11)	C43—C44	1.502 (14)
C4—C9	1.523 (11)	C43—H43A	0.9900
C4—C5	1.530 (10)	C43—H43B	0.9900
C4—H4	1.0000	C44—C45	1.533 (13)
C5—C6	1.522 (11)	C44—H44A	0.9900
C5—H5A	0.9900	C44—H44B	0.9900
C5—H5B	0.9900	C45—C46	1.526 (11)
C6—C7	1.526 (12)	C45—H45A	0.9900
C6—H6A	0.9900	C45—H45B	0.9900
C6—H6B	0.9900	C46—H46A	0.9900
C7—C8	1.516 (12)	C46—H46B	0.9900
C7—H7A	0.9900	C47—N10	1.349 (10)
C7—H7B	0.9900	C47—C48	1.376 (11)
C8—C9	1.536 (10)	C47—H47	0.9500
C8—H8A	0.9900	C48—C49	1.378 (10)
C8—H8B	0.9900	C48—H48	0.9500
C9—H9A	0.9900	C49—N9	1.327 (10)
C9—H9B	0.9900	C49—C50	1.490 (11)
C10—N4	1.338 (10)	C50—C55	1.524 (11)
C10—C11	1.368 (11)	C50—C51	1.527 (11)
C10—H10	0.9500	C50—H50	1.0000
C11—C12	1.407 (10)	C51—C52	1.522 (12)
C11—H11	0.9500	C51—H51A	0.9900
C12—N3	1.349 (10)	C51—H51B	0.9900
C12—C13	1.494 (10)	C52—C53	1.516 (12)
C13—C14	1.524 (11)	C52—H52A	0.9900
C13—C18	1.528 (11)	C52—H52B	0.9900
C13—H13	1.0000	C53—C54	1.512 (11)
C14—C15	1.518 (11)	C53—H53A	0.9900
C14—H14A	0.9900	C53—H53B	0.9900
C14—H14B	0.9900	C54—C55	1.514 (11)
C15—C16	1.528 (11)	C54—H54A	0.9900
C15—H15A	0.9900	C54—H54B	0.9900
C15—H15B	0.9900	C55—H55A	0.9900
C16—C17	1.508 (11)	C55—H55B	0.9900
C16—H16A	0.9900	C56—N12	1.348 (10)
C16—H16B	0.9900	C56—C57	1.356 (11)
C17—C18	1.525 (11)	C56—H56	0.9500
C17—H17A	0.9900	C57—C58	1.402 (10)
C17—H17B	0.9900	C57—H57	0.9500
C18—H18A	0.9900	C58—N11	1.351 (10)
C18—H18B	0.9900	C58—C59	1.488 (11)
C19—N6	1.353 (9)	C59—C60	1.522 (10)
C19—C20	1.384 (11)	C59—C64	1.552 (10)
C19—H19	0.9500	C59—H59	1.0000
C20—C21	1.395 (11)	C60—C61	1.521 (11)
C20—H20	0.9500	C60—H60A	0.9900
C21—N5	1.347 (10)	C60—H60B	0.9900
C21—C22	1.490 (10)	C61—C62	1.536 (12)
C22—C23	1.521 (11)	C61—H61A	0.9900
C22—C27	1.541 (11)	C61—H61B	0.9900
C22—H22	1.0000	C62—C63	1.513 (12)
C23—C24	1.525 (11)	C62—H62A	0.9900
C23—H23A	0.9900	C62—H62B	0.9900
C23—H23B	0.9900	C63—C64	1.507 (11)
C24—C25	1.510 (12)	C63—H63A	0.9900
C24—H24A	0.9900	C63—H63B	0.9900
C24—H24B	0.9900	C64—H64A	0.9900
C25—C26	1.534 (12)	C64—H64B	0.9900
C25—H25A	0.9900	C65—N13	1.140 (13)
C25—H25B	0.9900	C65—C66	1.455 (14)
C26—C27	1.512 (11)	C66—H66A	0.9800
C26—H26A	0.9900	C66—H66B	0.9800
C26—H26B	0.9900	C66—H66C	0.9800
C27—H27A	0.9900	Co1—O1	1.987 (5)
C27—H27B	0.9900	Co1—O2	1.990 (5)
C28—C29	1.499 (10)	Co1—N1	2.059 (6)
C28—H28A	0.9800	Co1—N5	2.094 (7)
C28—H28B	0.9800	Co1—N3	2.114 (6)
C28—H28C	0.9800	Co2—O3	1.985 (5)
C29—O1	1.283 (8)	Co2—O4	1.990 (5)
C29—C30	1.418 (10)	Co2—N11	2.057 (6)
C30—C31	1.413 (10)	Co2—N7	2.093 (7)
C30—C35	1.501 (7)	Co2—N9	2.120 (6)
C31—O2	1.269 (9)	N1—N2	1.365 (8)
C31—C32	1.510 (11)	N3—N4	1.364 (8)
C32—H32A	0.9800	N5—N6	1.351 (8)
C32—H32B	0.9800	N7—N8	1.361 (9)
C32—H32C	0.9800	N9—N10	1.358 (8)
C33—C34	1.523 (10)	N11—N12	1.353 (9)
C33—H33A	0.9800	N14—C67	1.138 (15)
C33—H33B	0.9800	C67—C68	1.49 (3)
C33—H33C	0.9800	C68—H68A	0.9800
C34—O4	1.261 (8)	C68—H68B	0.9800
C34—C35	1.413 (10)	C68—H68C	0.9800
C35—C36	1.394 (10)	N14B—C67B	1.15 (2)
C36—O3	1.282 (9)	C67B—C68B	1.49 (3)
C36—C37	1.512 (10)	C68B—H68D	0.9800
C37—H37A	0.9800	C68B—H68E	0.9800
C37—H37B	0.9800	C68B—H68F	0.9800
N2—B1—N6	109.6 (6)	C42—C41—H41	108.0
N2—B1—N4	109.2 (6)	C43—C42—C41	110.0 (8)
N6—B1—N4	106.0 (6)	C43—C42—H42A	109.7
N2—B1—H1A	110.7	C41—C42—H42A	109.7
N6—B1—H1A	110.7	C43—C42—H42B	109.7
N4—B1—H1A	110.7	C41—C42—H42B	109.7
N12—B2—N10	108.8 (7)	H42A—C42—H42B	108.2
N12—B2—N8	109.9 (7)	C44—C43—C42	111.4 (8)
N10—B2—N8	105.8 (6)	C44—C43—H43A	109.3
N12—B2—H2A	110.7	C42—C43—H43A	109.3
N10—B2—H2A	110.7	C44—C43—H43B	109.3
N8—B2—H2A	110.7	C42—C43—H43B	109.3
N2—C1—C2	108.4 (7)	H43A—C43—H43B	108.0
N2—C1—H1	125.8	C43—C44—C45	110.2 (7)
C2—C1—H1	125.8	C43—C44—H44A	109.6
C1—C2—C3	105.9 (7)	C45—C44—H44A	109.6
C1—C2—H2	127.0	C43—C44—H44B	109.6
C3—C2—H2	127.0	C45—C44—H44B	109.6
N1—C3—C2	108.7 (7)	H44A—C44—H44B	108.1
N1—C3—C4	120.7 (7)	C46—C45—C44	110.2 (8)
C2—C3—C4	130.6 (7)	C46—C45—H45A	109.6
C3—C4—C9	111.3 (6)	C44—C45—H45A	109.6
C3—C4—C5	111.9 (6)	C46—C45—H45B	109.6
C9—C4—C5	110.9 (7)	C44—C45—H45B	109.6
C3—C4—H4	107.5	H45A—C45—H45B	108.1
C9—C4—H4	107.5	C41—C46—C45	112.2 (7)
C5—C4—H4	107.5	C41—C46—H46A	109.2
C6—C5—C4	111.3 (6)	C45—C46—H46A	109.2
C6—C5—H5A	109.4	C41—C46—H46B	109.2
C4—C5—H5A	109.4	C45—C46—H46B	109.2
C6—C5—H5B	109.4	H46A—C46—H46B	107.9
C4—C5—H5B	109.4	N10—C47—C48	107.4 (7)
H5A—C5—H5B	108.0	N10—C47—H47	126.3
C5—C6—C7	111.6 (7)	C48—C47—H47	126.3
C5—C6—H6A	109.3	C47—C48—C49	106.0 (7)
C7—C6—H6A	109.3	C47—C48—H48	127.0
C5—C6—H6B	109.3	C49—C48—H48	127.0
C7—C6—H6B	109.3	N9—C49—C48	110.0 (7)
H6A—C6—H6B	108.0	N9—C49—C50	121.7 (7)
C8—C7—C6	111.7 (7)	C48—C49—C50	128.4 (7)
C8—C7—H7A	109.3	C49—C50—C55	112.5 (6)
C6—C7—H7A	109.3	C49—C50—C51	110.6 (7)
C8—C7—H7B	109.3	C55—C50—C51	110.9 (6)
C6—C7—H7B	109.3	C49—C50—H50	107.6
H7A—C7—H7B	107.9	C55—C50—H50	107.6
C7—C8—C9	111.3 (7)	C51—C50—H50	107.6
C7—C8—H8A	109.4	C52—C51—C50	111.6 (7)
C9—C8—H8A	109.4	C52—C51—H51A	109.3
C7—C8—H8B	109.4	C50—C51—H51A	109.3
C9—C8—H8B	109.4	C52—C51—H51B	109.3
H8A—C8—H8B	108.0	C50—C51—H51B	109.3
C4—C9—C8	110.5 (6)	H51A—C51—H51B	108.0
C4—C9—H9A	109.5	C53—C52—C51	110.8 (7)
C8—C9—H9A	109.5	C53—C52—H52A	109.5
C4—C9—H9B	109.5	C51—C52—H52A	109.5
C8—C9—H9B	109.5	C53—C52—H52B	109.5
H9A—C9—H9B	108.1	C51—C52—H52B	109.5
N4—C10—C11	109.4 (7)	H52A—C52—H52B	108.1
N4—C10—H10	125.3	C54—C53—C52	110.5 (7)
C11—C10—H10	125.3	C54—C53—H53A	109.6
C10—C11—C12	104.8 (7)	C52—C53—H53A	109.6
C10—C11—H11	127.6	C54—C53—H53B	109.6
C12—C11—H11	127.6	C52—C53—H53B	109.6
N3—C12—C11	109.6 (7)	H53A—C53—H53B	108.1
N3—C12—C13	120.8 (6)	C53—C54—C55	111.6 (7)
C11—C12—C13	129.7 (7)	C53—C54—H54A	109.3
C12—C13—C14	111.5 (6)	C55—C54—H54A	109.3
C12—C13—C18	111.0 (7)	C53—C54—H54B	109.3
C14—C13—C18	110.9 (6)	C55—C54—H54B	109.3
C12—C13—H13	107.7	H54A—C54—H54B	108.0
C14—C13—H13	107.7	C54—C55—C50	111.3 (7)
C18—C13—H13	107.7	C54—C55—H55A	109.4
C15—C14—C13	110.9 (7)	C50—C55—H55A	109.4
C15—C14—H14A	109.5	C54—C55—H55B	109.4
C13—C14—H14A	109.5	C50—C55—H55B	109.4
C15—C14—H14B	109.5	H55A—C55—H55B	108.0
C13—C14—H14B	109.5	N12—C56—C57	109.1 (7)
H14A—C14—H14B	108.0	N12—C56—H56	125.5
C14—C15—C16	110.9 (7)	C57—C56—H56	125.5
C14—C15—H15A	109.5	C56—C57—C58	105.6 (7)
C16—C15—H15A	109.5	C56—C57—H57	127.2
C14—C15—H15B	109.5	C58—C57—H57	127.2
C16—C15—H15B	109.5	N11—C58—C57	108.9 (7)
H15A—C15—H15B	108.0	N11—C58—C59	120.2 (6)
C17—C16—C15	111.1 (7)	C57—C58—C59	130.8 (7)
C17—C16—H16A	109.4	C58—C59—C60	112.7 (6)
C15—C16—H16A	109.4	C58—C59—C64	111.0 (6)
C17—C16—H16B	109.4	C60—C59—C64	109.1 (6)
C15—C16—H16B	109.4	C58—C59—H59	108.0
H16A—C16—H16B	108.0	C60—C59—H59	108.0
C16—C17—C18	111.0 (7)	C64—C59—H59	108.0
C16—C17—H17A	109.4	C61—C60—C59	112.5 (7)
C18—C17—H17A	109.4	C61—C60—H60A	109.1
C16—C17—H17B	109.4	C59—C60—H60A	109.1
C18—C17—H17B	109.4	C61—C60—H60B	109.1
H17A—C17—H17B	108.0	C59—C60—H60B	109.1
C17—C18—C13	111.0 (7)	H60A—C60—H60B	107.8
C17—C18—H18A	109.4	C60—C61—C62	110.7 (7)
C13—C18—H18A	109.4	C60—C61—H61A	109.5
C17—C18—H18B	109.4	C62—C61—H61A	109.5
C13—C18—H18B	109.4	C60—C61—H61B	109.5
H18A—C18—H18B	108.0	C62—C61—H61B	109.5
N6—C19—C20	108.1 (7)	H61A—C61—H61B	108.1
N6—C19—H19	125.9	C63—C62—C61	111.2 (7)
C20—C19—H19	125.9	C63—C62—H62A	109.4
C19—C20—C21	105.4 (7)	C61—C62—H62A	109.4
C19—C20—H20	127.3	C63—C62—H62B	109.4
C21—C20—H20	127.3	C61—C62—H62B	109.4
N5—C21—C20	109.3 (6)	H62A—C62—H62B	108.0
N5—C21—C22	120.4 (7)	C64—C63—C62	112.0 (7)
C20—C21—C22	130.3 (7)	C64—C63—H63A	109.2
C21—C22—C23	113.1 (6)	C62—C63—H63A	109.2
C21—C22—C27	110.6 (6)	C64—C63—H63B	109.2
C23—C22—C27	109.5 (6)	C62—C63—H63B	109.2
C21—C22—H22	107.9	H63A—C63—H63B	107.9
C23—C22—H22	107.9	C63—C64—C59	111.3 (6)
C27—C22—H22	107.9	C63—C64—H64A	109.4
C22—C23—C24	110.9 (7)	C59—C64—H64A	109.4
C22—C23—H23A	109.5	C63—C64—H64B	109.4
C24—C23—H23A	109.5	C59—C64—H64B	109.4
C22—C23—H23B	109.5	H64A—C64—H64B	108.0
C24—C23—H23B	109.5	N13—C65—C66	178.1 (10)
H23A—C23—H23B	108.0	C65—C66—H66A	109.5
C25—C24—C23	112.0 (7)	C65—C66—H66B	109.5
C25—C24—H24A	109.2	H66A—C66—H66B	109.5
C23—C24—H24A	109.2	C65—C66—H66C	109.5
C25—C24—H24B	109.2	H66A—C66—H66C	109.5
C23—C24—H24B	109.2	H66B—C66—H66C	109.5
H24A—C24—H24B	107.9	O1—Co1—O2	86.3 (2)
C24—C25—C26	109.5 (7)	O1—Co1—N1	106.5 (2)
C24—C25—H25A	109.8	O2—Co1—N1	102.4 (2)
C26—C25—H25A	109.8	O1—Co1—N5	92.5 (2)
C24—C25—H25B	109.8	O2—Co1—N5	167.4 (2)
C26—C25—H25B	109.8	N1—Co1—N5	90.1 (2)
H25A—C25—H25B	108.2	O1—Co1—N3	163.1 (2)
C27—C26—C25	111.5 (7)	O2—Co1—N3	94.1 (2)
C27—C26—H26A	109.3	N1—Co1—N3	89.9 (2)
C25—C26—H26A	109.3	N5—Co1—N3	83.5 (2)
C27—C26—H26B	109.3	O3—Co2—O4	86.7 (2)
C25—C26—H26B	109.3	O3—Co2—N11	106.8 (2)
H26A—C26—H26B	108.0	O4—Co2—N11	101.9 (2)
C26—C27—C22	111.9 (6)	O3—Co2—N7	92.8 (2)
C26—C27—H27A	109.2	O4—Co2—N7	167.2 (2)
C22—C27—H27A	109.2	N11—Co2—N7	90.5 (2)
C26—C27—H27B	109.2	O3—Co2—N9	163.0 (2)
C22—C27—H27B	109.2	O4—Co2—N9	93.3 (2)
H27A—C27—H27B	107.9	N11—Co2—N9	89.8 (2)
C29—C28—H28A	109.5	N7—Co2—N9	83.5 (2)
C29—C28—H28B	109.5	C3—N1—N2	107.8 (6)
H28A—C28—H28B	109.5	C3—N1—Co1	134.5 (5)
C29—C28—H28C	109.5	N2—N1—Co1	117.3 (5)
H28A—C28—H28C	109.5	C1—N2—N1	109.1 (7)
H28B—C28—H28C	109.5	C1—N2—B1	130.3 (7)
O1—C29—C30	124.3 (7)	N1—N2—B1	120.5 (6)
O1—C29—C28	114.5 (7)	C12—N3—N4	106.4 (6)
C30—C29—C28	121.0 (6)	C12—N3—Co1	136.9 (5)
C31—C30—C29	121.2 (6)	N4—N3—Co1	116.5 (5)
C31—C30—C35	118.3 (7)	C10—N4—N3	109.7 (6)
C29—C30—C35	120.4 (7)	C10—N4—B1	130.2 (7)
O2—C31—C30	125.4 (7)	N3—N4—B1	120.1 (6)
O2—C31—C32	114.4 (6)	C21—N5—N6	107.6 (6)
C30—C31—C32	120.1 (6)	C21—N5—Co1	135.8 (5)
C31—C32—H32A	109.5	N6—N5—Co1	116.5 (5)
C31—C32—H32B	109.5	N5—N6—C19	109.5 (6)
H32A—C32—H32B	109.5	N5—N6—B1	120.8 (6)
C31—C32—H32C	109.5	C19—N6—B1	128.9 (6)
H32A—C32—H32C	109.5	C40—N7—N8	107.4 (7)
H32B—C32—H32C	109.5	C40—N7—Co2	136.3 (5)
C34—C33—H33A	109.5	N8—N7—Co2	116.1 (5)
C34—C33—H33B	109.5	C38—N8—N7	108.7 (6)
H33A—C33—H33B	109.5	C38—N8—B2	129.3 (7)
C34—C33—H33C	109.5	N7—N8—B2	120.4 (6)
H33A—C33—H33C	109.5	C49—N9—N10	107.0 (6)
H33B—C33—H33C	109.5	C49—N9—Co2	136.9 (5)
O4—C34—C35	126.4 (7)	N10—N9—Co2	116.0 (5)
O4—C34—C33	113.5 (6)	C47—N10—N9	109.5 (6)
C35—C34—C33	120.1 (6)	C47—N10—B2	129.8 (6)
C36—C35—C34	120.6 (6)	N9—N10—B2	120.6 (6)
C36—C35—C30	121.8 (7)	C58—N11—N12	107.0 (6)
C34—C35—C30	117.6 (7)	C58—N11—Co2	134.6 (5)
O3—C36—C35	125.8 (7)	N12—N11—Co2	117.8 (5)
O3—C36—C37	113.2 (6)	C56—N12—N11	109.4 (7)
C35—C36—C37	121.0 (6)	C56—N12—B2	130.1 (7)
C36—C37—H37A	109.5	N11—N12—B2	120.3 (6)
C36—C37—H37B	109.5	C29—O1—Co1	128.9 (5)
H37A—C37—H37B	109.5	C31—O2—Co1	129.8 (5)
C36—C37—H37C	109.5	C36—O3—Co2	128.0 (5)
H37A—C37—H37C	109.5	C34—O4—Co2	128.6 (5)
H37B—C37—H37C	109.5	N14—C67—C68	179.1 (16)
N8—C38—C39	108.7 (7)	C67—C68—H68A	109.5
N8—C38—H38	125.7	C67—C68—H68B	109.5
C39—C38—H38	125.7	H68A—C68—H68B	109.5
C38—C39—C40	105.1 (7)	C67—C68—H68C	109.5
C38—C39—H39	127.5	H68A—C68—H68C	109.5
C40—C39—H39	127.5	H68B—C68—H68C	109.5
N7—C40—C39	110.2 (7)	N14B—C67B—C68B	174 (8)
N7—C40—C41	121.0 (7)	C67B—C68B—H68D	109.5
C39—C40—C41	128.7 (7)	C67B—C68B—H68E	109.5
C40—C41—C46	110.7 (6)	H68D—C68B—H68E	109.5
C40—C41—C42	112.6 (7)	C67B—C68B—H68F	109.5
C46—C41—C42	109.4 (7)	H68D—C68B—H68F	109.5
C40—C41—H41	108.0	H68E—C68B—H68F	109.5
C46—C41—H41	108.0
N2—C1—C2—C3	−0.9 (9)	C57—C58—C59—C64	74.3 (10)
C1—C2—C3—N1	0.2 (9)	C58—C59—C60—C61	180.0 (7)
C1—C2—C3—C4	−179.3 (8)	C64—C59—C60—C61	56.2 (8)
N1—C3—C4—C9	−98.6 (8)	C59—C60—C61—C62	−55.8 (9)
C2—C3—C4—C9	80.9 (10)	C60—C61—C62—C63	54.0 (9)
N1—C3—C4—C5	136.7 (7)	C61—C62—C63—C64	−55.2 (9)
C2—C3—C4—C5	−43.8 (11)	C62—C63—C64—C59	56.6 (9)
C3—C4—C5—C6	−178.9 (7)	C58—C59—C64—C63	179.2 (7)
C9—C4—C5—C6	56.2 (8)	C60—C59—C64—C63	−56.0 (8)
C4—C5—C6—C7	−54.4 (9)	C2—C3—N1—N2	0.6 (8)
C5—C6—C7—C8	53.9 (9)	C4—C3—N1—N2	−179.9 (6)
C6—C7—C8—C9	−54.8 (9)	C2—C3—N1—Co1	−171.9 (5)
C3—C4—C9—C8	177.9 (6)	C4—C3—N1—Co1	7.7 (11)
C5—C4—C9—C8	−56.8 (8)	C2—C1—N2—N1	1.2 (9)
C7—C8—C9—C4	56.3 (9)	C2—C1—N2—B1	177.7 (7)
N4—C10—C11—C12	1.1 (9)	C3—N1—N2—C1	−1.1 (8)
C10—C11—C12—N3	0.8 (9)	Co1—N1—N2—C1	172.9 (5)
C10—C11—C12—C13	180.0 (8)	C3—N1—N2—B1	−178.0 (7)
N3—C12—C13—C14	116.3 (8)	Co1—N1—N2—B1	−4.0 (8)
C11—C12—C13—C14	−62.8 (11)	N6—B1—N2—C1	129.3 (8)
N3—C12—C13—C18	−119.5 (8)	N4—B1—N2—C1	−115.0 (8)
C11—C12—C13—C18	61.4 (11)	N6—B1—N2—N1	−54.5 (9)
C12—C13—C14—C15	−179.9 (7)	N4—B1—N2—N1	61.2 (8)
C18—C13—C14—C15	55.8 (9)	C11—C12—N3—N4	−2.3 (8)
C13—C14—C15—C16	−56.2 (9)	C13—C12—N3—N4	178.4 (6)
C14—C15—C16—C17	56.7 (9)	C11—C12—N3—Co1	−177.8 (6)
C15—C16—C17—C18	−56.4 (9)	C13—C12—N3—Co1	3.0 (12)
C16—C17—C18—C13	55.9 (9)	C11—C10—N4—N3	−2.6 (9)
C12—C13—C18—C17	179.9 (6)	C11—C10—N4—B1	174.9 (8)
C14—C13—C18—C17	−55.5 (9)	C12—N3—N4—C10	3.0 (8)
N6—C19—C20—C21	1.1 (9)	Co1—N3—N4—C10	179.6 (5)
C19—C20—C21—N5	−1.5 (9)	C12—N3—N4—B1	−174.8 (6)
C19—C20—C21—C22	174.3 (7)	Co1—N3—N4—B1	1.8 (9)
N5—C21—C22—C23	−175.0 (7)	N2—B1—N4—C10	123.8 (8)
C20—C21—C22—C23	9.6 (11)	N6—B1—N4—C10	−118.3 (8)
N5—C21—C22—C27	61.9 (9)	N2—B1—N4—N3	−58.9 (9)
C20—C21—C22—C27	−113.6 (9)	N6—B1—N4—N3	59.0 (9)
C21—C22—C23—C24	−179.6 (6)	C20—C21—N5—N6	1.4 (8)
C27—C22—C23—C24	−55.9 (8)	C22—C21—N5—N6	−174.9 (6)
C22—C23—C24—C25	58.3 (9)	C20—C21—N5—Co1	179.2 (6)
C23—C24—C25—C26	−56.7 (10)	C22—C21—N5—Co1	2.9 (11)
C24—C25—C26—C27	55.6 (9)	C21—N5—N6—C19	−0.7 (8)
C25—C26—C27—C22	−56.0 (9)	Co1—N5—N6—C19	−179.0 (5)
C21—C22—C27—C26	−179.2 (6)	C21—N5—N6—B1	170.2 (7)
C23—C22—C27—C26	55.6 (9)	Co1—N5—N6—B1	−8.1 (8)
O1—C29—C30—C31	2.0 (12)	C20—C19—N6—N5	−0.3 (8)
C28—C29—C30—C31	178.0 (7)	C20—C19—N6—B1	−170.2 (7)
O1—C29—C30—C35	178.3 (7)	N2—B1—N6—N5	62.0 (9)
C28—C29—C30—C35	−5.7 (11)	N4—B1—N6—N5	−55.7 (9)
C29—C30—C31—O2	6.2 (12)	N2—B1—N6—C19	−129.0 (8)
C35—C30—C31—O2	−170.1 (7)	N4—B1—N6—C19	113.3 (8)
C29—C30—C31—C32	−173.0 (7)	C39—C40—N7—N8	0.0 (9)
C35—C30—C31—C32	10.7 (10)	C41—C40—N7—N8	−175.9 (7)
O4—C34—C35—C36	8.4 (12)	C39—C40—N7—Co2	174.7 (6)
C33—C34—C35—C36	−171.5 (7)	C41—C40—N7—Co2	−1.2 (12)
O4—C34—C35—C30	−171.8 (7)	C39—C38—N8—N7	−0.2 (9)
C33—C34—C35—C30	8.4 (10)	C39—C38—N8—B2	−165.8 (7)
C31—C30—C35—C36	−107.3 (9)	C40—N7—N8—C38	0.1 (8)
C29—C30—C35—C36	76.4 (8)	Co2—N7—N8—C38	−175.8 (5)
C31—C30—C35—C34	72.9 (7)	C40—N7—N8—B2	167.2 (7)
C29—C30—C35—C34	−103.5 (9)	Co2—N7—N8—B2	−8.7 (8)
C34—C35—C36—O3	−1.6 (12)	N12—B2—N8—C38	−133.7 (8)
C30—C35—C36—O3	178.5 (7)	N10—B2—N8—C38	109.0 (9)
C34—C35—C36—C37	176.2 (7)	N12—B2—N8—N7	62.2 (9)
C30—C35—C36—C37	−3.6 (11)	N10—B2—N8—N7	−55.2 (9)
N8—C38—C39—C40	0.2 (9)	C48—C49—N9—N10	−2.8 (9)
C38—C39—C40—N7	−0.2 (9)	C50—C49—N9—N10	178.2 (7)
C38—C39—C40—C41	175.4 (8)	C48—C49—N9—Co2	179.6 (6)
N7—C40—C41—C46	60.2 (10)	C50—C49—N9—Co2	0.6 (12)
C39—C40—C41—C46	−114.9 (9)	C48—C47—N10—N9	−1.2 (9)
N7—C40—C41—C42	−177.0 (7)	C48—C47—N10—B2	176.3 (8)
C39—C40—C41—C42	7.9 (12)	C49—N9—N10—C47	2.5 (9)
C40—C41—C42—C43	179.4 (7)	Co2—N9—N10—C47	−179.3 (5)
C46—C41—C42—C43	−57.1 (9)	C49—N9—N10—B2	−175.3 (7)
C41—C42—C43—C44	59.4 (10)	Co2—N9—N10—B2	2.9 (9)
C42—C43—C44—C45	−58.5 (10)	N12—B2—N10—C47	122.9 (8)
C43—C44—C45—C46	55.9 (10)	N8—B2—N10—C47	−119.0 (8)
C40—C41—C46—C45	−178.9 (7)	N12—B2—N10—N9	−59.8 (9)
C42—C41—C46—C45	56.5 (9)	N8—B2—N10—N9	58.3 (9)
C44—C45—C46—C41	−55.9 (10)	C57—C58—N11—N12	0.4 (8)
N10—C47—C48—C49	−0.6 (9)	C59—C58—N11—N12	179.2 (6)
C47—C48—C49—N9	2.1 (9)	C57—C58—N11—Co2	−170.4 (6)
C47—C48—C49—C50	−179.0 (8)	C59—C58—N11—Co2	8.3 (11)
N9—C49—C50—C55	116.2 (8)	C57—C56—N12—N11	1.7 (9)
C48—C49—C50—C55	−62.6 (11)	C57—C56—N12—B2	177.3 (8)
N9—C49—C50—C51	−119.2 (8)	C58—N11—N12—C56	−1.3 (8)
C48—C49—C50—C51	62.0 (11)	Co2—N11—N12—C56	171.3 (5)
C49—C50—C51—C52	−179.7 (7)	C58—N11—N12—B2	−177.4 (7)
C55—C50—C51—C52	−54.2 (9)	Co2—N11—N12—B2	−4.8 (9)
C50—C51—C52—C53	55.9 (9)	N10—B2—N12—C56	−113.6 (8)
C51—C52—C53—C54	−56.9 (10)	N8—B2—N12—C56	131.0 (8)
C52—C53—C54—C55	57.2 (10)	N10—B2—N12—N11	61.7 (9)
C53—C54—C55—C50	−55.9 (10)	N8—B2—N12—N11	−53.8 (9)
C49—C50—C55—C54	178.3 (7)	C30—C29—O1—Co1	−20.5 (11)
C51—C50—C55—C54	53.9 (9)	C28—C29—O1—Co1	163.3 (5)
N12—C56—C57—C58	−1.4 (9)	C30—C31—O2—Co1	4.4 (11)
C56—C57—C58—N11	0.6 (9)	C32—C31—O2—Co1	−176.3 (5)
C56—C57—C58—C59	−178.0 (8)	C35—C36—O3—Co2	−17.3 (11)
N11—C58—C59—C60	133.2 (7)	C37—C36—O3—Co2	164.7 (5)
C57—C58—C59—C60	−48.4 (11)	C35—C34—O4—Co2	4.5 (11)
N11—C58—C59—C64	−104.1 (8)	C33—C34—O4—Co2	−175.7 (5)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C10—H10···N14B^i	0.95	2.44	3.31 (4)	152
C13—H13···O2	1.00	2.49	3.302 (9)	138
C22—H22···O1	1.00	2.46	3.186 (9)	129
C41—H41···O3	1.00	2.56	3.229 (9)	125
C50—H50···O4	1.00	2.51	3.295 (9)	135

Symmetry code: (i) x, y+1, z.

(II) (µ-3,4-Diacetylhexa-2,4-diene-2,5-diolato-κ⁴O²,O³:O⁴,O⁵)bis{[tris(3-neopentyl-1H-pyrazol-1-yl-κN²)borato]nickel(II)}

Crystal data

[Ni2(C24H40BN6)2(C10H12O4)]	Dx = 1.228 Mg m^−3
Mr = 1160.47	Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, Fdd2	Cell parameters from 2424 reflections
a = 19.630 (3) Å	θ = 2.5–30.5°
b = 61.387 (10) Å	µ = 0.65 mm^−1
c = 10.4220 (17) Å	T = 100 K
V = 12559 (3) Å^3	Plate, green
Z = 8	0.55 × 0.35 × 0.18 mm
F(000) = 4976

Data collection

Bruker SMART APEX CCD diffractometer	6859 independent reflections
Radiation source: fine-focus sealed tube	6456 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.021
ω scans	θmax = 31.5°, θmin = 2.2°
Absorption correction: multi-scan (APEX2; Bruker, 2009)	h = −22→28
Tmin = 0.609, Tmax = 0.746	k = −83→81
14135 measured reflections	l = −10→15

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) = 0.071	w = 1/[σ^2(Fo^2) + (0.0386P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.02	(Δ/σ)max = 0.001
6859 reflections	Δρmax = 0.47 e Å^−3
363 parameters	Δρmin = −0.25 e Å^−3
1 restraint	Absolute structure: Flack x determined using 1695 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.014 (6)

Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

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

	x	y	z	Uiso*/Ueq
B1	0.37055 (12)	0.10916 (4)	0.5864 (3)	0.0219 (5)
H1A	0.3581	0.1248	0.5754	0.026*
C1	0.47381 (12)	0.11648 (4)	0.4340 (2)	0.0267 (5)
H1	0.4635	0.1310	0.4097	0.032*
C2	0.52857 (11)	0.10444 (4)	0.3913 (2)	0.0270 (5)
H2	0.5627	0.1089	0.3324	0.032*
C3	0.52324 (10)	0.08436 (3)	0.4529 (2)	0.0188 (4)
C4	0.57074 (10)	0.06531 (4)	0.4512 (2)	0.0191 (4)
H4A	0.5807	0.0614	0.3609	0.023*
H4B	0.5477	0.0527	0.4912	0.023*
C5	0.63898 (10)	0.06946 (4)	0.5222 (2)	0.0231 (4)
C6	0.62526 (12)	0.07878 (4)	0.6556 (2)	0.0295 (5)
H6A	0.6040	0.0931	0.6474	0.044*
H6B	0.6683	0.0802	0.7024	0.044*
H6C	0.5947	0.0690	0.7025	0.044*
C7	0.68441 (12)	0.08515 (4)	0.4467 (3)	0.0348 (6)
H7A	0.7286	0.0865	0.4898	0.052*
H7B	0.6625	0.0995	0.4423	0.052*
H7C	0.6913	0.0795	0.3597	0.052*
C8	0.67610 (11)	0.04760 (4)	0.5353 (3)	0.0301 (5)
H8A	0.6475	0.0374	0.5833	0.045*
H8B	0.7192	0.0498	0.5810	0.045*
H8C	0.6854	0.0417	0.4498	0.045*
C9	0.25174 (11)	0.09967 (4)	0.4912 (2)	0.0281 (5)
H9	0.2342	0.1140	0.4810	0.034*
C10	0.21725 (11)	0.08056 (4)	0.4659 (2)	0.0282 (5)
H10	0.1719	0.0791	0.4352	0.034*
C11	0.26302 (10)	0.06371 (4)	0.4948 (2)	0.0200 (4)
C12	0.25217 (10)	0.03965 (4)	0.4824 (2)	0.0204 (4)
H12A	0.2957	0.0329	0.4558	0.024*
H12B	0.2188	0.0371	0.4128	0.024*
C13	0.22668 (10)	0.02784 (4)	0.6043 (2)	0.0208 (4)
C14	0.15758 (10)	0.03700 (4)	0.6446 (2)	0.0269 (5)
H14A	0.1624	0.0525	0.6662	0.040*
H14B	0.1409	0.0290	0.7197	0.040*
H14C	0.1251	0.0354	0.5738	0.040*
C15	0.27762 (11)	0.03029 (4)	0.7140 (2)	0.0255 (5)
H15A	0.2619	0.0219	0.7882	0.038*
H15B	0.2813	0.0457	0.7378	0.038*
H15C	0.3223	0.0249	0.6865	0.038*
C16	0.21881 (13)	0.00371 (4)	0.5716 (3)	0.0341 (6)
H16A	0.2036	−0.0042	0.6479	0.051*
H16B	0.2627	−0.0021	0.5429	0.051*
H16C	0.1851	0.0020	0.5031	0.051*
C17	0.36068 (12)	0.11557 (4)	0.8318 (3)	0.0275 (5)
H17	0.3488	0.1306	0.8308	0.033*
C18	0.36290 (12)	0.10255 (4)	0.9386 (2)	0.0283 (5)
H18	0.3533	0.1067	1.0246	0.034*
C19	0.38236 (9)	0.08187 (4)	0.8942 (2)	0.0189 (4)
C20	0.39073 (11)	0.06090 (4)	0.9647 (2)	0.0217 (4)
H20A	0.4110	0.0501	0.9051	0.026*
H20B	0.3449	0.0555	0.9881	0.026*
C21	0.43480 (12)	0.06150 (4)	1.0878 (2)	0.0274 (5)
C22	0.50163 (12)	0.07339 (5)	1.0612 (3)	0.0355 (6)
H22A	0.5318	0.0720	1.1356	0.053*
H22B	0.4923	0.0888	1.0453	0.053*
H22C	0.5236	0.0670	0.9857	0.053*
C23	0.39712 (16)	0.07195 (7)	1.1994 (3)	0.0492 (8)
H23A	0.3928	0.0876	1.1843	0.074*
H23B	0.4226	0.0695	1.2790	0.074*
H23C	0.3517	0.0655	1.2070	0.074*
C24	0.45045 (14)	0.03787 (5)	1.1239 (3)	0.0422 (7)
H24A	0.4769	0.0376	1.2037	0.063*
H24B	0.4768	0.0310	1.0551	0.063*
H24C	0.4077	0.0299	1.1361	0.063*
C25	0.41526 (10)	0.00150 (3)	0.4107 (2)	0.0184 (4)
H25A	0.4394	0.0042	0.3299	0.028*
H25B	0.3661	0.0031	0.3969	0.028*
H25C	0.4250	−0.0133	0.4404	0.028*
C26	0.43874 (9)	0.01771 (3)	0.51069 (18)	0.0139 (3)
C27	0.48565 (8)	0.01132 (3)	0.60721 (19)	0.0139 (3)
C28	0.50625 (9)	0.02637 (3)	0.70239 (18)	0.0152 (4)
C29	0.56187 (11)	0.02021 (4)	0.7966 (2)	0.0225 (4)
H29A	0.5417	0.0127	0.8702	0.034*
H29B	0.5852	0.0334	0.8262	0.034*
H29C	0.5947	0.0106	0.7542	0.034*
N1	0.43755 (9)	0.10416 (3)	0.51571 (19)	0.0208 (4)
N2	0.46739 (8)	0.08416 (3)	0.52719 (17)	0.0165 (3)
N3	0.31409 (9)	0.09451 (3)	0.5326 (2)	0.0226 (4)
N4	0.32183 (8)	0.07232 (3)	0.53559 (18)	0.0183 (3)
N5	0.37796 (8)	0.10367 (3)	0.72915 (19)	0.0205 (4)
N6	0.39141 (8)	0.08273 (3)	0.76695 (18)	0.0172 (3)
Ni1	0.41180 (2)	0.06133 (2)	0.61902 (2)	0.01362 (6)
O1	0.41345 (6)	0.03656 (2)	0.49760 (14)	0.0157 (3)
O2	0.48155 (7)	0.04526 (2)	0.71942 (14)	0.0169 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
B1	0.0235 (10)	0.0151 (12)	0.0273 (13)	0.0042 (8)	0.0004 (9)	0.0024 (9)
C1	0.0329 (11)	0.0168 (12)	0.0305 (12)	−0.0013 (9)	0.0029 (9)	0.0075 (9)
C2	0.0306 (10)	0.0240 (12)	0.0264 (13)	−0.0032 (9)	0.0073 (9)	0.0059 (9)
C3	0.0220 (9)	0.0179 (10)	0.0164 (9)	−0.0043 (7)	0.0024 (7)	−0.0011 (8)
C4	0.0204 (8)	0.0178 (10)	0.0191 (10)	−0.0031 (7)	0.0029 (7)	−0.0036 (8)
C5	0.0196 (9)	0.0227 (11)	0.0270 (11)	−0.0031 (8)	0.0029 (8)	−0.0071 (9)
C6	0.0279 (10)	0.0300 (13)	0.0306 (13)	−0.0049 (9)	−0.0035 (9)	−0.0105 (10)
C7	0.0275 (10)	0.0325 (14)	0.0445 (16)	−0.0110 (10)	0.0106 (11)	−0.0076 (12)
C8	0.0199 (9)	0.0300 (13)	0.0405 (14)	0.0005 (9)	−0.0020 (9)	−0.0074 (11)
C9	0.0251 (10)	0.0262 (13)	0.0330 (13)	0.0101 (9)	−0.0028 (9)	0.0079 (10)
C10	0.0212 (9)	0.0340 (14)	0.0293 (12)	0.0049 (9)	−0.0071 (9)	0.0092 (10)
C11	0.0178 (8)	0.0292 (12)	0.0132 (9)	0.0012 (8)	−0.0021 (7)	0.0024 (8)
C12	0.0173 (8)	0.0270 (12)	0.0169 (9)	−0.0008 (8)	−0.0014 (7)	−0.0034 (8)
C13	0.0190 (8)	0.0229 (11)	0.0206 (11)	0.0000 (7)	0.0026 (8)	−0.0021 (9)
C14	0.0208 (9)	0.0352 (14)	0.0248 (12)	0.0007 (8)	0.0047 (8)	−0.0008 (10)
C15	0.0234 (9)	0.0326 (13)	0.0205 (10)	0.0023 (9)	0.0002 (8)	0.0052 (9)
C16	0.0362 (12)	0.0255 (13)	0.0407 (14)	−0.0037 (10)	0.0106 (11)	−0.0046 (11)
C17	0.0272 (10)	0.0186 (12)	0.0367 (13)	0.0028 (8)	0.0043 (9)	−0.0086 (10)
C18	0.0311 (11)	0.0279 (13)	0.0259 (12)	0.0023 (9)	0.0050 (9)	−0.0111 (10)
C19	0.0173 (8)	0.0224 (11)	0.0169 (10)	−0.0010 (7)	−0.0007 (7)	−0.0053 (8)
C20	0.0234 (9)	0.0281 (13)	0.0137 (9)	−0.0023 (8)	−0.0002 (8)	0.0002 (8)
C21	0.0247 (10)	0.0415 (15)	0.0159 (10)	−0.0046 (9)	−0.0029 (8)	0.0034 (10)
C22	0.0237 (11)	0.0444 (17)	0.0382 (15)	−0.0065 (10)	−0.0079 (10)	0.0068 (12)
C23	0.0472 (15)	0.083 (3)	0.0174 (12)	−0.0084 (16)	−0.0008 (11)	−0.0104 (15)
C24	0.0433 (13)	0.0500 (17)	0.0334 (13)	−0.0113 (12)	−0.0130 (12)	0.0224 (14)
C25	0.0219 (9)	0.0162 (10)	0.0170 (9)	−0.0007 (7)	−0.0044 (7)	−0.0015 (8)
C26	0.0152 (7)	0.0138 (9)	0.0126 (8)	−0.0008 (6)	0.0017 (6)	0.0014 (7)
C27	0.0146 (7)	0.0140 (9)	0.0131 (8)	0.0020 (6)	0.0012 (6)	0.0007 (7)
C28	0.0159 (8)	0.0154 (10)	0.0144 (9)	0.0006 (7)	−0.0003 (7)	0.0019 (7)
C29	0.0266 (10)	0.0183 (11)	0.0224 (10)	0.0045 (8)	−0.0106 (8)	−0.0022 (8)
N1	0.0238 (8)	0.0153 (9)	0.0233 (9)	0.0021 (7)	0.0015 (7)	0.0053 (7)
N2	0.0196 (7)	0.0119 (8)	0.0181 (8)	0.0012 (6)	−0.0004 (6)	0.0004 (6)
N3	0.0226 (8)	0.0184 (9)	0.0267 (9)	0.0050 (7)	−0.0020 (7)	0.0052 (8)
N4	0.0192 (7)	0.0175 (9)	0.0182 (8)	0.0023 (6)	−0.0018 (6)	0.0028 (7)
N5	0.0211 (8)	0.0143 (9)	0.0261 (10)	0.0036 (6)	0.0019 (7)	−0.0011 (7)
N6	0.0194 (7)	0.0125 (8)	0.0196 (8)	0.0017 (6)	−0.0007 (6)	−0.0005 (7)
Ni1	0.01520 (9)	0.01223 (11)	0.01345 (10)	0.00120 (9)	−0.00035 (9)	0.00088 (10)
O1	0.0174 (6)	0.0156 (7)	0.0142 (7)	0.0013 (5)	−0.0019 (5)	0.0008 (5)
O2	0.0202 (6)	0.0142 (7)	0.0163 (7)	0.0033 (5)	−0.0030 (5)	−0.0017 (6)

Geometric parameters (Å, º)

B1—N5	1.533 (3)	C16—H16B	0.9800
B1—N3	1.533 (3)	C16—H16C	0.9800
B1—N1	1.538 (3)	C17—N5	1.339 (3)
B1—H1A	1.0000	C17—C18	1.371 (4)
C1—N1	1.343 (3)	C17—H17	0.9500
C1—C2	1.378 (3)	C18—C19	1.405 (3)
C1—H1	0.9500	C18—H18	0.9500
C2—C3	1.393 (3)	C19—N6	1.339 (3)
C2—H2	0.9500	C19—C20	1.491 (3)
C3—N2	1.342 (3)	C20—C21	1.548 (3)
C3—C4	1.496 (3)	C20—H20A	0.9900
C4—C5	1.552 (3)	C20—H20B	0.9900
C4—H4A	0.9900	C21—C23	1.520 (4)
C4—H4B	0.9900	C21—C22	1.527 (3)
C5—C6	1.527 (3)	C21—C24	1.530 (4)
C5—C7	1.530 (3)	C22—H22A	0.9800
C5—C8	1.533 (3)	C22—H22B	0.9800
C6—H6A	0.9800	C22—H22C	0.9800
C6—H6B	0.9800	C23—H23A	0.9800
C6—H6C	0.9800	C23—H23B	0.9800
C7—H7A	0.9800	C23—H23C	0.9800
C7—H7B	0.9800	C24—H24A	0.9800
C7—H7C	0.9800	C24—H24B	0.9800
C8—H8A	0.9800	C24—H24C	0.9800
C8—H8B	0.9800	C25—C26	1.513 (3)
C8—H8C	0.9800	C25—H25A	0.9800
C9—N3	1.336 (3)	C25—H25B	0.9800
C9—C10	1.380 (4)	C25—H25C	0.9800
C9—H9	0.9500	C26—O1	1.267 (2)
C10—C11	1.403 (3)	C26—C27	1.419 (3)
C10—H10	0.9500	C27—C28	1.415 (3)
C11—N4	1.339 (3)	C27—C27^i	1.499 (4)
C11—C12	1.498 (3)	C28—O2	1.269 (2)
C12—C13	1.545 (3)	C28—C29	1.516 (3)
C12—H12A	0.9900	C29—H29A	0.9800
C12—H12B	0.9900	C29—H29B	0.9800
C13—C15	1.526 (3)	C29—H29C	0.9800
C13—C14	1.527 (3)	N1—N2	1.365 (2)
C13—C16	1.528 (3)	N2—Ni1	2.0177 (17)
C14—H14A	0.9800	N3—N4	1.371 (3)
C14—H14B	0.9800	N4—Ni1	2.0810 (17)
C14—H14C	0.9800	N5—N6	1.370 (3)
C15—H15A	0.9800	N6—Ni1	2.0645 (18)
C15—H15B	0.9800	Ni1—O1	1.9785 (15)
C15—H15C	0.9800	Ni1—O2	1.9856 (14)
C16—H16A	0.9800
N5—B1—N3	107.09 (19)	C17—C18—C19	105.6 (2)
N5—B1—N1	109.85 (17)	C17—C18—H18	127.2
N3—B1—N1	109.02 (19)	C19—C18—H18	127.2
N5—B1—H1A	110.3	N6—C19—C18	109.1 (2)
N3—B1—H1A	110.3	N6—C19—C20	120.49 (19)
N1—B1—H1A	110.3	C18—C19—C20	130.4 (2)
N1—C1—C2	108.4 (2)	C19—C20—C21	116.74 (19)
N1—C1—H1	125.8	C19—C20—H20A	108.1
C2—C1—H1	125.8	C21—C20—H20A	108.1
C1—C2—C3	105.48 (19)	C19—C20—H20B	108.1
C1—C2—H2	127.3	C21—C20—H20B	108.1
C3—C2—H2	127.3	H20A—C20—H20B	107.3
N2—C3—C2	109.59 (19)	C23—C21—C22	110.8 (2)
N2—C3—C4	120.59 (19)	C23—C21—C24	108.1 (2)
C2—C3—C4	129.73 (19)	C22—C21—C24	109.0 (2)
C3—C4—C5	113.81 (18)	C23—C21—C20	111.9 (2)
C3—C4—H4A	108.8	C22—C21—C20	109.91 (19)
C5—C4—H4A	108.8	C24—C21—C20	107.1 (2)
C3—C4—H4B	108.8	C21—C22—H22A	109.5
C5—C4—H4B	108.8	C21—C22—H22B	109.5
H4A—C4—H4B	107.7	H22A—C22—H22B	109.5
C6—C5—C7	109.6 (2)	C21—C22—H22C	109.5
C6—C5—C8	109.3 (2)	H22A—C22—H22C	109.5
C7—C5—C8	108.65 (19)	H22B—C22—H22C	109.5
C6—C5—C4	110.09 (17)	C21—C23—H23A	109.5
C7—C5—C4	111.2 (2)	C21—C23—H23B	109.5
C8—C5—C4	107.98 (18)	H23A—C23—H23B	109.5
C5—C6—H6A	109.5	C21—C23—H23C	109.5
C5—C6—H6B	109.5	H23A—C23—H23C	109.5
H6A—C6—H6B	109.5	H23B—C23—H23C	109.5
C5—C6—H6C	109.5	C21—C24—H24A	109.5
H6A—C6—H6C	109.5	C21—C24—H24B	109.5
H6B—C6—H6C	109.5	H24A—C24—H24B	109.5
C5—C7—H7A	109.5	C21—C24—H24C	109.5
C5—C7—H7B	109.5	H24A—C24—H24C	109.5
H7A—C7—H7B	109.5	H24B—C24—H24C	109.5
C5—C7—H7C	109.5	C26—C25—H25A	109.5
H7A—C7—H7C	109.5	C26—C25—H25B	109.5
H7B—C7—H7C	109.5	H25A—C25—H25B	109.5
C5—C8—H8A	109.5	C26—C25—H25C	109.5
C5—C8—H8B	109.5	H25A—C25—H25C	109.5
H8A—C8—H8B	109.5	H25B—C25—H25C	109.5
C5—C8—H8C	109.5	O1—C26—C27	125.68 (18)
H8A—C8—H8C	109.5	O1—C26—C25	114.03 (17)
H8B—C8—H8C	109.5	C27—C26—C25	120.28 (18)
N3—C9—C10	108.0 (2)	C28—C27—C26	120.12 (17)
N3—C9—H9	126.0	C28—C27—C27^i	119.86 (14)
C10—C9—H9	126.0	C26—C27—C27^i	120.01 (15)
C9—C10—C11	105.74 (19)	O2—C28—C27	125.85 (17)
C9—C10—H10	127.1	O2—C28—C29	114.37 (18)
C11—C10—H10	127.1	C27—C28—C29	119.78 (18)
N4—C11—C10	109.2 (2)	C28—C29—H29A	109.5
N4—C11—C12	122.64 (18)	C28—C29—H29B	109.5
C10—C11—C12	128.12 (19)	H29A—C29—H29B	109.5
C11—C12—C13	115.98 (18)	C28—C29—H29C	109.5
C11—C12—H12A	108.3	H29A—C29—H29C	109.5
C13—C12—H12A	108.3	H29B—C29—H29C	109.5
C11—C12—H12B	108.3	C1—N1—N2	109.54 (18)
C13—C12—H12B	108.3	C1—N1—B1	130.09 (19)
H12A—C12—H12B	107.4	N2—N1—B1	120.30 (18)
C15—C13—C14	109.82 (19)	C3—N2—N1	106.95 (17)
C15—C13—C16	109.2 (2)	C3—N2—Ni1	136.21 (15)
C14—C13—C16	109.18 (18)	N1—N2—Ni1	115.72 (12)
C15—C13—C12	110.92 (16)	C9—N3—N4	110.16 (19)
C14—C13—C12	109.95 (18)	C9—N3—B1	129.9 (2)
C16—C13—C12	107.74 (18)	N4—N3—B1	119.65 (17)
C13—C14—H14A	109.5	C11—N4—N3	106.84 (17)
C13—C14—H14B	109.5	C11—N4—Ni1	137.41 (15)
H14A—C14—H14B	109.5	N3—N4—Ni1	115.19 (13)
C13—C14—H14C	109.5	C17—N5—N6	109.33 (19)
H14A—C14—H14C	109.5	C17—N5—B1	129.2 (2)
H14B—C14—H14C	109.5	N6—N5—B1	120.26 (18)
C13—C15—H15A	109.5	C19—N6—N5	107.22 (18)
C13—C15—H15B	109.5	C19—N6—Ni1	137.75 (15)
H15A—C15—H15B	109.5	N5—N6—Ni1	114.80 (14)
C13—C15—H15C	109.5	O1—Ni1—O2	86.79 (6)
H15A—C15—H15C	109.5	O1—Ni1—N2	102.80 (7)
H15B—C15—H15C	109.5	O2—Ni1—N2	102.82 (6)
C13—C16—H16A	109.5	O1—Ni1—N6	165.87 (6)
C13—C16—H16B	109.5	O2—Ni1—N6	93.22 (6)
H16A—C16—H16B	109.5	N2—Ni1—N6	90.98 (7)
C13—C16—H16C	109.5	O1—Ni1—N4	89.77 (6)
H16A—C16—H16C	109.5	O2—Ni1—N4	165.14 (7)
H16B—C16—H16C	109.5	N2—Ni1—N4	92.04 (7)
N5—C17—C18	108.8 (2)	N6—Ni1—N4	86.63 (7)
N5—C17—H17	125.6	C26—O1—Ni1	129.77 (13)
C18—C17—H17	125.6	C28—O2—Ni1	130.05 (13)
N1—C1—C2—C3	−0.5 (3)	C4—C3—N2—N1	175.53 (18)
C1—C2—C3—N2	1.1 (3)	C2—C3—N2—Ni1	165.56 (17)
C1—C2—C3—C4	−175.3 (2)	C4—C3—N2—Ni1	−17.7 (3)
N2—C3—C4—C5	−106.7 (2)	C1—N1—N2—C3	0.9 (2)
C2—C3—C4—C5	69.3 (3)	B1—N1—N2—C3	178.23 (19)
C3—C4—C5—C6	50.0 (3)	C1—N1—N2—Ni1	−168.98 (15)
C3—C4—C5—C7	−71.7 (2)	B1—N1—N2—Ni1	8.3 (2)
C3—C4—C5—C8	169.25 (19)	C10—C9—N3—N4	−0.1 (3)
N3—C9—C10—C11	0.0 (3)	C10—C9—N3—B1	−173.3 (2)
C9—C10—C11—N4	0.1 (3)	N5—B1—N3—C9	111.1 (3)
C9—C10—C11—C12	−178.9 (2)	N1—B1—N3—C9	−130.1 (2)
N4—C11—C12—C13	87.5 (2)	N5—B1—N3—N4	−61.5 (2)
C10—C11—C12—C13	−93.6 (3)	N1—B1—N3—N4	57.3 (3)
C11—C12—C13—C15	−60.7 (2)	C10—C11—N4—N3	−0.2 (2)
C11—C12—C13—C14	61.0 (2)	C12—C11—N4—N3	178.88 (19)
C11—C12—C13—C16	179.87 (18)	C10—C11—N4—Ni1	170.40 (18)
N5—C17—C18—C19	−0.3 (3)	C12—C11—N4—Ni1	−10.5 (3)
C17—C18—C19—N6	0.2 (2)	C9—N3—N4—C11	0.2 (2)
C17—C18—C19—C20	−177.4 (2)	B1—N3—N4—C11	174.1 (2)
N6—C19—C20—C21	132.3 (2)	C9—N3—N4—Ni1	−172.80 (16)
C18—C19—C20—C21	−50.3 (3)	B1—N3—N4—Ni1	1.2 (2)
C19—C20—C21—C23	75.4 (3)	C18—C17—N5—N6	0.3 (2)
C19—C20—C21—C22	−48.1 (3)	C18—C17—N5—B1	167.3 (2)
C19—C20—C21—C24	−166.4 (2)	N3—B1—N5—C17	−109.2 (2)
O1—C26—C27—C28	2.2 (3)	N1—B1—N5—C17	132.6 (2)
C25—C26—C27—C28	−178.51 (17)	N3—B1—N5—N6	56.6 (2)
O1—C26—C27—C27^i	−176.77 (18)	N1—B1—N5—N6	−61.7 (2)
C25—C26—C27—C27^i	2.5 (3)	C18—C19—N6—N5	−0.1 (2)
C26—C27—C28—O2	7.4 (3)	C20—C19—N6—N5	177.82 (17)
C27^i—C27—C28—O2	−173.57 (18)	C18—C19—N6—Ni1	−174.13 (16)
C26—C27—C28—C29	−173.53 (18)	C20—C19—N6—Ni1	3.7 (3)
C27^i—C27—C28—C29	5.5 (3)	C17—N5—N6—C19	−0.1 (2)
C2—C1—N1—N2	−0.2 (3)	B1—N5—N6—C19	−168.47 (17)
C2—C1—N1—B1	−177.2 (2)	C17—N5—N6—Ni1	175.48 (14)
N5—B1—N1—C1	−130.8 (2)	B1—N5—N6—Ni1	7.1 (2)
N3—B1—N1—C1	112.1 (3)	C27—C26—O1—Ni1	−14.9 (3)
N5—B1—N1—N2	52.4 (3)	C25—C26—O1—Ni1	165.82 (12)
N3—B1—N1—N2	−64.6 (2)	C27—C28—O2—Ni1	−4.0 (3)
C2—C3—N2—N1	−1.2 (2)	C29—C28—O2—Ni1	176.93 (14)

Symmetry code: (i) −x+1, −y, z.