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Acta Cryst. (2007). E63, m1905    [ doi:10.1107/S1600536807028371 ]

A tetranuclear nickel(II) cluster: bis[[mu]3-2,6-bis(methylamino)pyridine(2-)-[kappa]4N2:N1,N6:N6]bis[[mu]3-2,6-bis(methylamino)pyridine(1-)-[kappa]3N1:N2:N2]dichloridotetranickel(II)

F. A. Cotton, C. A. Murillo and Q. Wang

Abstract top

The title compound, [Ni4(C7H9N3)2(C7H10N3)2Cl2], was obtained from a reaction in which 2,6-dimethylaminopyridine, in the presence of methyllithium used to deprotonate the organic ligand precursor, was added to NiCl2 during an attempt to synthesize a linear trinuclear nickel chain. During this reaction, two equivalents of the amine were fully deprotonated, forming dianions, and the three N atoms coordinate to Ni centers. The other two equivalents of the amine were only partially deprotonated, giving monoanions in which only two N atoms coordinate to Ni centers. In this tetranuclear complex, two of the four Ni atoms have square-planar coordination and are bonded to four N donors, while the other two are in a distorted tetrahedral geometry, with three coordination sites occupied by N donors and the fourth by a Cl atom. The molecule is noncentrosymmetic but the crystal structure is racemic.

Comment top

Molecules in the title complex, (I) (Fig. 1), are non-centrosymmetic but the crystals are racemic. During the reaction, two equivalents of the organic amine were fully deprotonated forming dianions and two equivalents were only partially deprotonated giving monoanions. In this tetranuclear complex, there are four divalent Ni atoms. Two of them, Ni1 and Ni4, are square planar and bonded to four N donors while the others, Ni2 and Ni3, are in a distorted tetrahedral geometry, with three coordination sites occupied by N donors and the fourth one by a Cl atom (Table 1). Even though there are a series of compounds having three Ni atoms forming a linear chain that have both four-coordinate and five-coordinate metal atoms (Clérac et al., 1999; Cotton et al., 2001, 2006), examples of clusters having four Ni atoms in a four-coordinate environment but two different geometries are rare.

Related literature top

For related structures, see: Clérac et al. (1999); Cotton et al. (2001, 2006).

Experimental top

Compound (I) was obtained by adding 2 equivalents of CH3Li (2 mmol) to deprotonate a THF solution (15 ml) of the organic amine, 2,6-dimethylaminopyridine (0.137 g, 1 mmol), at 195 K. This mixture was then transferred via cannula to solid, anhydrous NiCl2 (0.130 g, 1 mmol). After stirring the mixture at room temperature for 5 h, the solvent was removed under vacuum. The brown solid was extracted with CH2Cl2 (10 ml). To this solution was added a layer of hexanes (30 ml). After a week at room temperature, large block-shaped, deep brown crystals were isolated.

Refinement top

All H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.94 Å (CH) and 0.97 Å (CH3), Uiso(H) = 1.2Ueq(C) and 1.5Ueq(C), and N—H = 0.87 Å, Uiso(H) = 1.2Ueq(N).

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. The molecular structure of (I). Displacement ellipsoids are drawn at the 40% probability level. H atoms have been omitted for clarity.
[Figure 2] Fig. 2. The packing diagram of (I).
bis[µ3-2,6-bis(methylamino)pyridine(2-)-κ4N2:N1,N6:N6]bis[µ3– 2,6-bis(methylamino)pyridine(1-)-κ3N1:N2:N2]dichloridotetranickel(II) top
Crystal data top
[Ni4(C7H9N3)2(C7H10N3)2Cl2]F000 = 1744
Mr = 848.44Dx = 1.669 Mg m−3
Monoclinic, P21/cMo Kα radiation
λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5894 reflections
a = 12.710 (7) Åθ = 2.5–25.0º
b = 10.903 (6) ŵ = 2.40 mm−1
c = 24.729 (14) ÅT = 213 (2) K
β = 99.842 (11)ºBlock, brown
V = 3376 (3) Å30.38 × 0.10 × 0.10 mm
Z = 4
Data collection top
Bruker SMART 1000 area-detector
diffractometer		5894 independent reflections
Radiation source: fine-focus sealed tube4026 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.057
T = 213(2) Kθmax = 25.0º
φ and ω scansθmin = 2.5º
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −15→15
Tmin = 0.463, Tmax = 0.796k = −12→9
16834 measured reflectionsl = −29→29
Refinement top
Refinement on F2H-atom parameters constrained
Least-squares matrix: full  w = 1/[σ2(Fo2) + (0.033P)2 + 0.98P]
where P = (Fo2 + 2Fc2)/3
R[F2 > 2σ(F2)] = 0.042(Δ/σ)max = 0.001
wR(F2) = 0.094Δρmax = 0.66 e Å−3
S = 1.08Δρmin = −0.57 e Å−3
5894 reflectionsExtinction correction: none
415 parameters
Crystal data top
[Ni4(C7H9N3)2(C7H10N3)2Cl2]V = 3376 (3) Å3
Mr = 848.44Z = 4
Monoclinic, P21/cMo Kα
a = 12.710 (7) ŵ = 2.40 mm−1
b = 10.903 (6) ÅT = 213 (2) K
c = 24.729 (14) Å0.38 × 0.10 × 0.10 mm
β = 99.842 (11)º
Data collection top
Bruker SMART 1000 area-detector
diffractometer		5894 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		4026 reflections with I > 2σ(I)
Tmin = 0.463, Tmax = 0.796Rint = 0.057
16834 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.042415 parameters
wR(F2) = 0.094H-atom parameters constrained
S = 1.08Δρmax = 0.66 e Å−3
5894 reflectionsΔρmin = −0.57 e Å−3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.85881 (5)0.60891 (5)0.15069 (2)0.02005 (16)
Ni20.69244 (5)0.44549 (6)0.08446 (2)0.02496 (17)
Ni30.78862 (5)0.84198 (6)0.22024 (2)0.02465 (17)
Ni40.68609 (5)0.74121 (6)0.11001 (2)0.02360 (16)
Cl10.69651 (12)0.30291 (14)0.01981 (6)0.0501 (4)
Cl20.82948 (11)1.02671 (12)0.25863 (6)0.0431 (4)
N90.7045 (3)0.6199 (3)0.05452 (14)0.0229 (9)
N10.8208 (3)0.4386 (4)0.14373 (14)0.0236 (9)
N60.5910 (3)0.6543 (4)0.14663 (15)0.0275 (10)
N110.8911 (3)0.7805 (3)0.17005 (14)0.0214 (9)
N80.8902 (3)0.6215 (3)0.07831 (14)0.0211 (9)
N50.6492 (3)0.8413 (4)0.16761 (15)0.0265 (10)
C120.7661 (4)0.3467 (5)0.22874 (18)0.0266 (11)
H12A0.75980.26510.21630.032*
C450.8823 (4)0.8608 (4)0.12564 (19)0.0244 (11)
C350.8042 (4)0.6318 (4)0.03666 (18)0.0211 (11)
N30.7878 (3)0.7147 (4)0.27437 (15)0.0281 (10)
C410.7679 (4)0.9352 (5)0.0482 (2)0.0342 (13)
C150.7818 (4)0.5948 (5)0.26349 (18)0.0261 (12)
C310.9908 (4)0.6291 (4)0.06617 (18)0.0224 (11)
C340.8177 (4)0.6542 (4)−0.01643 (18)0.0271 (12)
H34A0.75840.6600−0.04480.033*
N71.0728 (3)0.6098 (4)0.10788 (15)0.0282 (10)
H7A1.05830.58470.13920.034*
N20.8066 (3)0.5571 (4)0.21415 (14)0.0224 (9)
N100.7866 (3)0.8578 (3)0.09147 (15)0.0247 (9)
C330.9199 (4)0.6679 (5)−0.02711 (19)0.0313 (13)
H33A0.92970.6859−0.06310.038*
C10.8999 (4)0.3439 (5)0.1353 (2)0.0347 (13)
H1A0.95950.34610.16550.052*
H1B0.92550.36000.10120.052*
H1C0.86660.26370.13350.052*
C40.6031 (4)0.9650 (5)0.1564 (2)0.0421 (15)
H4A0.53620.95880.13100.063*
H4B0.65251.01580.14050.063*
H4C0.59021.00160.19050.063*
C80.9947 (3)0.7864 (4)0.20777 (19)0.0271 (12)
H8A1.05120.75920.18870.041*
H8B0.99240.73380.23920.041*
H8C1.00840.87020.22020.041*
C60.6110 (4)0.6238 (5)0.00933 (18)0.0300 (12)
H6A0.60780.7032−0.00860.045*
H6B0.54610.61070.02420.045*
H6C0.61800.5600−0.01720.045*
C210.5402 (4)0.5453 (5)0.14940 (18)0.0263 (11)
C130.7460 (4)0.3815 (5)0.28017 (19)0.0308 (13)
H13A0.72700.32090.30370.037*
C321.0067 (4)0.6562 (5)0.01277 (18)0.0291 (12)
H32A1.07590.66600.00480.035*
C220.4607 (4)0.5417 (5)0.18400 (19)0.0325 (13)
H22A0.42110.46980.18660.039*
C420.8451 (5)1.0147 (5)0.0362 (2)0.0456 (15)
H42A0.83121.06690.00560.055*
C110.7955 (3)0.4397 (5)0.19779 (18)0.0231 (11)
N40.5677 (3)0.4520 (4)0.12021 (15)0.0271 (10)
C250.5747 (4)0.7504 (5)0.17780 (19)0.0301 (12)
C140.7529 (4)0.4998 (5)0.29750 (19)0.0312 (13)
H14A0.73830.51920.33250.037*
C51.1831 (4)0.6287 (5)0.1031 (2)0.0371 (14)
H5A1.22830.60970.13780.056*
H5B1.19370.71360.09360.056*
H5C1.20160.57550.07470.056*
C20.7635 (5)0.7497 (5)0.32769 (19)0.0450 (15)
H2A0.76600.67770.35090.068*
H2B0.69270.78560.32300.068*
H2C0.81560.80920.34470.068*
C230.4429 (4)0.6434 (6)0.2131 (2)0.0408 (15)
H23A0.38970.64010.23520.049*
C440.9628 (4)0.9405 (5)0.1151 (2)0.0347 (13)
H44A1.02940.94250.13850.042*
C240.5000 (4)0.7520 (5)0.2116 (2)0.0372 (14)
H24A0.48810.82130.23230.045*
C70.6361 (6)0.9856 (6)−0.0350 (2)0.084 (3)
H7B0.56100.9703−0.04860.126*
H7C0.67860.9510−0.06030.126*
H7D0.64851.0733−0.03190.126*
N120.6660 (4)0.9295 (4)0.01813 (18)0.0474 (13)
H12B0.61740.89000.03200.057*
C30.5172 (4)0.3343 (5)0.1267 (2)0.0370 (13)
H3A0.45600.34640.14480.055*
H3B0.56800.28020.14870.055*
H3C0.49380.29770.09090.055*
C430.9424 (5)1.0160 (5)0.0698 (2)0.0478 (16)
H43A0.99611.06900.06190.057*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0208 (3)0.0221 (4)0.0173 (3)−0.0009 (3)0.0035 (2)−0.0001 (3)
Ni20.0246 (3)0.0261 (4)0.0238 (3)−0.0024 (3)0.0032 (3)−0.0022 (3)
Ni30.0248 (3)0.0252 (4)0.0231 (3)0.0019 (3)0.0016 (3)−0.0030 (3)
Ni40.0203 (3)0.0264 (4)0.0230 (3)0.0010 (3)0.0007 (3)−0.0012 (3)
Cl10.0583 (9)0.0478 (10)0.0442 (8)0.0032 (8)0.0088 (7)−0.0205 (7)
Cl20.0510 (9)0.0275 (8)0.0484 (8)−0.0018 (7)0.0018 (7)−0.0116 (6)
N90.022 (2)0.025 (2)0.021 (2)−0.002 (2)0.0005 (17)−0.0003 (17)
N10.023 (2)0.026 (2)0.022 (2)−0.002 (2)0.0049 (17)−0.0030 (18)
N60.022 (2)0.037 (3)0.022 (2)0.001 (2)0.0009 (17)−0.0017 (19)
N110.023 (2)0.021 (2)0.020 (2)0.0011 (19)0.0014 (16)0.0014 (17)
N80.025 (2)0.023 (2)0.016 (2)−0.0025 (19)0.0048 (17)−0.0027 (16)
N50.024 (2)0.029 (2)0.025 (2)0.003 (2)0.0012 (18)−0.0068 (19)
C120.027 (3)0.022 (3)0.030 (3)−0.005 (2)0.000 (2)0.007 (2)
C450.029 (3)0.016 (3)0.028 (3)0.002 (2)0.005 (2)−0.002 (2)
C350.025 (3)0.016 (3)0.022 (2)−0.001 (2)0.004 (2)−0.003 (2)
N30.035 (2)0.029 (3)0.023 (2)0.002 (2)0.0104 (19)−0.0047 (19)
C410.046 (3)0.023 (3)0.031 (3)0.004 (3)0.001 (3)0.005 (2)
C150.020 (2)0.040 (4)0.017 (2)0.005 (3)0.001 (2)0.004 (2)
C310.026 (3)0.019 (3)0.024 (3)−0.001 (2)0.008 (2)−0.001 (2)
C340.033 (3)0.029 (3)0.019 (3)0.000 (3)0.003 (2)0.004 (2)
N70.018 (2)0.043 (3)0.025 (2)−0.001 (2)0.0056 (17)0.002 (2)
N20.024 (2)0.025 (2)0.019 (2)0.002 (2)0.0069 (17)0.0009 (18)
N100.027 (2)0.019 (2)0.027 (2)0.005 (2)−0.0003 (18)0.0015 (18)
C330.041 (3)0.035 (3)0.020 (3)−0.004 (3)0.012 (2)0.004 (2)
C10.034 (3)0.038 (3)0.034 (3)0.008 (3)0.009 (2)−0.003 (3)
C40.042 (3)0.043 (4)0.037 (3)0.015 (3)−0.004 (3)−0.006 (3)
C80.020 (2)0.028 (3)0.031 (3)−0.001 (2)−0.003 (2)−0.002 (2)
C60.029 (3)0.035 (3)0.024 (3)−0.003 (3)−0.002 (2)−0.001 (2)
C210.020 (3)0.035 (3)0.022 (3)−0.003 (3)−0.002 (2)−0.001 (2)
C130.026 (3)0.038 (4)0.027 (3)−0.003 (3)0.000 (2)0.017 (2)
C320.031 (3)0.032 (3)0.027 (3)−0.004 (3)0.012 (2)0.000 (2)
C220.017 (3)0.047 (4)0.033 (3)0.000 (3)0.006 (2)0.005 (3)
C420.070 (4)0.030 (3)0.036 (3)−0.003 (3)0.007 (3)0.012 (3)
C110.013 (2)0.033 (3)0.022 (2)0.006 (2)−0.0010 (19)−0.001 (2)
N40.024 (2)0.028 (3)0.029 (2)−0.005 (2)0.0031 (18)0.000 (2)
C250.023 (3)0.039 (3)0.028 (3)0.002 (3)0.001 (2)−0.002 (2)
C140.029 (3)0.043 (4)0.022 (3)0.003 (3)0.007 (2)0.007 (2)
C50.024 (3)0.055 (4)0.032 (3)−0.001 (3)0.006 (2)−0.002 (3)
C20.065 (4)0.045 (4)0.027 (3)0.006 (3)0.016 (3)−0.003 (3)
C230.026 (3)0.070 (4)0.030 (3)0.008 (3)0.015 (2)0.003 (3)
C440.029 (3)0.031 (3)0.045 (3)−0.008 (3)0.009 (2)0.002 (3)
C240.025 (3)0.052 (4)0.036 (3)0.008 (3)0.007 (2)−0.004 (3)
C70.127 (7)0.061 (5)0.043 (4)−0.002 (5)−0.045 (4)0.020 (3)
N120.055 (3)0.041 (3)0.040 (3)0.002 (3)−0.012 (2)0.013 (2)
C30.037 (3)0.045 (4)0.030 (3)−0.010 (3)0.007 (2)0.001 (3)
C430.052 (4)0.032 (4)0.063 (4)−0.017 (3)0.022 (3)0.006 (3)
Geometric parameters (Å, °) top
Ni1—N21.891 (4)N7—H7A0.8700
Ni1—N81.904 (4)N2—C111.343 (6)
Ni1—N11.919 (4)C33—C321.354 (6)
Ni1—N111.957 (4)C33—H33A0.9400
Ni1—C112.393 (5)C1—H1A0.9700
Ni1—Ni42.6753 (14)C1—H1B0.9700
Ni2—N41.945 (4)C1—H1C0.9700
Ni2—N12.000 (4)C4—H4A0.9700
Ni2—N92.056 (4)C4—H4B0.9700
Ni2—Cl12.2369 (17)C4—H4C0.9700
Ni3—N31.929 (4)C8—H8A0.9700
Ni3—N52.012 (4)C8—H8B0.9700
Ni3—N112.059 (4)C8—H8C0.9700
Ni3—Cl22.2492 (18)C6—H6A0.9700
Ni4—N61.885 (4)C6—H6B0.9700
Ni4—N101.913 (4)C6—H6C0.9700
Ni4—N51.915 (4)C21—N41.328 (6)
Ni4—N91.948 (4)C21—C221.432 (6)
Ni4—C252.374 (5)C13—C141.357 (7)
N9—C351.417 (5)C13—H13A0.9400
N9—C61.487 (5)C32—H32A0.9400
N1—C111.427 (5)C22—C231.362 (7)
N1—C11.480 (6)C22—H22A0.9400
N6—C251.337 (6)C42—C431.366 (8)
N6—C211.360 (6)C42—H42A0.9400
N11—C451.394 (6)N4—C31.456 (6)
N11—C81.479 (5)C25—C241.369 (6)
N8—C311.365 (5)C14—H14A0.9400
N8—C351.372 (5)C5—H5A0.9700
N5—C251.423 (6)C5—H5B0.9700
N5—C41.478 (6)C5—H5C0.9700
C12—C111.361 (6)C2—H2A0.9700
C12—C131.392 (6)C2—H2B0.9700
C12—H12A0.9400C2—H2C0.9700
C45—N101.357 (6)C23—C241.393 (7)
C45—C441.401 (6)C23—H23A0.9400
C35—C341.375 (6)C44—C431.378 (7)
N3—C151.334 (6)C44—H44A0.9400
N3—C21.456 (5)C24—H24A0.9400
C41—N101.352 (6)C7—N121.440 (7)
C41—N121.379 (6)C7—H7B0.9700
C41—C421.379 (7)C7—H7C0.9700
C15—N21.374 (5)C7—H7D0.9700
C15—C141.422 (6)N12—H12B0.8700
C31—N71.352 (6)C3—H3A0.9700
C31—C321.401 (6)C3—H3B0.9700
C34—C331.377 (6)C3—H3C0.9700
C34—H34A0.9400C43—H43A0.9400
N7—C51.442 (5)
N2—Ni1—N8163.92 (17)C41—N10—C45119.7 (4)
N2—Ni1—N170.54 (16)C41—N10—Ni4124.7 (3)
N8—Ni1—N194.31 (15)C45—N10—Ni4115.5 (3)
N2—Ni1—N1199.85 (16)C32—C33—C34121.8 (4)
N8—Ni1—N1195.30 (15)C32—C33—H33A119.1
N1—Ni1—N11170.38 (15)C34—C33—H33A119.1
N2—Ni1—C1134.04 (15)N1—C1—H1A109.5
N8—Ni1—C11130.90 (16)N1—C1—H1B109.5
N1—Ni1—C1136.62 (15)H1A—C1—H1B109.5
N11—Ni1—C11133.77 (15)N1—C1—H1C109.5
N2—Ni1—Ni495.25 (12)H1A—C1—H1C109.5
N8—Ni1—Ni484.14 (12)H1B—C1—H1C109.5
N1—Ni1—Ni4108.08 (12)N5—C4—H4A109.5
N11—Ni1—Ni472.60 (11)N5—C4—H4B109.5
C11—Ni1—Ni4106.04 (11)H4A—C4—H4B109.5
N4—Ni2—N1107.15 (16)N5—C4—H4C109.5
N4—Ni2—N9104.29 (16)H4A—C4—H4C109.5
N1—Ni2—N9101.35 (15)H4B—C4—H4C109.5
N4—Ni2—Cl1118.08 (13)N11—C8—H8A109.5
N1—Ni2—Cl1112.46 (12)N11—C8—H8B109.5
N9—Ni2—Cl1111.92 (12)H8A—C8—H8B109.5
N3—Ni3—N5109.72 (17)N11—C8—H8C109.5
N3—Ni3—N11105.25 (16)H8A—C8—H8C109.5
N5—Ni3—N11100.78 (15)H8B—C8—H8C109.5
N3—Ni3—Cl2112.30 (13)N9—C6—H6A109.5
N5—Ni3—Cl2113.00 (12)N9—C6—H6B109.5
N11—Ni3—Cl2114.95 (11)H6A—C6—H6B109.5
N6—Ni4—N10163.47 (17)N9—C6—H6C109.5
N6—Ni4—N570.75 (17)H6A—C6—H6C109.5
N10—Ni4—N593.34 (17)H6B—C6—H6C109.5
N6—Ni4—N999.29 (17)N4—C21—N6118.1 (4)
N10—Ni4—N996.68 (16)N4—C21—C22125.6 (5)
N5—Ni4—N9169.96 (16)N6—C21—C22116.3 (5)
N6—Ni4—C2534.22 (17)C14—C13—C12122.4 (4)
N10—Ni4—C25130.15 (17)C14—C13—H13A118.8
N5—Ni4—C2536.81 (16)C12—C13—H13A118.8
N9—Ni4—C25133.15 (17)C33—C32—C31118.4 (4)
N6—Ni4—Ni195.77 (13)C33—C32—H32A120.8
N10—Ni4—Ni184.81 (12)C31—C32—H32A120.8
N5—Ni4—Ni1108.49 (12)C23—C22—C21119.5 (5)
N9—Ni4—Ni173.09 (11)C23—C22—H22A120.3
C25—Ni4—Ni1107.90 (12)C21—C22—H22A120.3
C35—N9—C6113.9 (3)C43—C42—C41118.7 (5)
C35—N9—Ni4112.3 (3)C43—C42—H42A120.7
C6—N9—Ni4109.5 (3)C41—C42—H42A120.7
C35—N9—Ni2108.8 (3)N2—C11—C12124.5 (4)
C6—N9—Ni2101.4 (3)N2—C11—N1105.2 (4)
Ni4—N9—Ni2110.41 (17)C12—C11—N1130.4 (5)
C11—N1—C1113.9 (4)N2—C11—Ni152.0 (2)
C11—N1—Ni190.1 (3)C12—C11—Ni1174.7 (4)
C1—N1—Ni1121.4 (3)N1—C11—Ni153.3 (2)
C11—N1—Ni2113.6 (3)C21—N4—C3117.0 (4)
C1—N1—Ni2114.3 (3)C21—N4—Ni2125.9 (3)
Ni1—N1—Ni2100.99 (18)C3—N4—Ni2115.3 (3)
C25—N6—C21122.2 (4)N6—C25—C24123.7 (5)
C25—N6—Ni493.4 (3)N6—C25—N5105.7 (4)
C21—N6—Ni4144.3 (3)C24—C25—N5130.7 (5)
C45—N11—C8114.4 (4)N6—C25—Ni452.4 (2)
C45—N11—Ni1115.0 (3)C24—C25—Ni4172.7 (4)
C8—N11—Ni1108.9 (3)N5—C25—Ni453.8 (2)
C45—N11—Ni3107.2 (3)C13—C14—C15121.0 (5)
C8—N11—Ni3101.1 (3)C13—C14—H14A119.5
Ni1—N11—Ni3109.33 (17)C15—C14—H14A119.5
C31—N8—C35119.0 (4)N7—C5—H5A109.5
C31—N8—Ni1124.4 (3)N7—C5—H5B109.5
C35—N8—Ni1116.3 (3)H5A—C5—H5B109.5
C25—N5—C4114.5 (4)N7—C5—H5C109.5
C25—N5—Ni489.4 (3)H5A—C5—H5C109.5
C4—N5—Ni4121.4 (3)H5B—C5—H5C109.5
C25—N5—Ni3115.3 (3)N3—C2—H2A109.5
C4—N5—Ni3113.3 (3)N3—C2—H2B109.5
Ni4—N5—Ni3100.52 (17)H2A—C2—H2B109.5
C11—C12—C13114.9 (5)N3—C2—H2C109.5
C11—C12—H12A122.5H2A—C2—H2C109.5
C13—C12—H12A122.5H2B—C2—H2C109.5
N10—C45—N11114.7 (4)C22—C23—C24122.9 (5)
N10—C45—C44120.3 (4)C22—C23—H23A118.5
N11—C45—C44125.0 (4)C24—C23—H23A118.5
N8—C35—C34121.2 (4)C43—C44—C45118.6 (5)
N8—C35—N9113.5 (4)C43—C44—H44A120.7
C34—C35—N9125.3 (4)C45—C44—H44A120.7
C15—N3—C2115.2 (4)C25—C24—C23115.1 (5)
C15—N3—Ni3124.9 (3)C25—C24—H24A122.4
C2—N3—Ni3117.8 (3)C23—C24—H24A122.4
N10—C41—N12114.9 (5)N12—C7—H7B109.5
N10—C41—C42121.7 (5)N12—C7—H7C109.5
N12—C41—C42123.3 (5)H7B—C7—H7C109.5
N3—C15—N2117.3 (4)N12—C7—H7D109.5
N3—C15—C14127.3 (4)H7B—C7—H7D109.5
N2—C15—C14115.4 (5)H7C—C7—H7D109.5
N7—C31—N8116.9 (4)C41—N12—C7123.4 (5)
N7—C31—C32122.4 (4)C41—N12—H12B118.3
N8—C31—C32120.8 (4)C7—N12—H12B118.3
C35—C34—C33118.6 (4)N4—C3—H3A109.5
C35—C34—H34A120.7N4—C3—H3B109.5
C33—C34—H34A120.7H3A—C3—H3B109.5
C31—N7—C5123.3 (4)N4—C3—H3C109.5
C31—N7—H7A118.4H3A—C3—H3C109.5
C5—N7—H7A118.4H3B—C3—H3C109.5
C11—N2—C15121.6 (4)C42—C43—C44120.8 (5)
C11—N2—Ni193.9 (3)C42—C43—H43A119.6
C15—N2—Ni1144.4 (4)C44—C43—H43A119.6
Table 1
Selected geometric parameters (Å) top
Ni1—N21.891 (4)Ni3—N31.929 (4)
Ni1—N81.904 (4)Ni3—N52.012 (4)
Ni1—N11.919 (4)Ni3—N112.059 (4)
Ni1—N111.957 (4)Ni3—Cl22.2492 (18)
Ni2—N41.945 (4)Ni4—N61.885 (4)
Ni2—N12.000 (4)Ni4—N101.913 (4)
Ni2—N92.056 (4)Ni4—N51.915 (4)
Ni2—Cl12.2369 (17)Ni4—N91.948 (4)
Acknowledgements top

The authors thank the Robert A. Welch Foundation and Texas A&M University for financial support.

references
References top

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