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The reddish-brown title complex, [Ni(C18H27N2Si)2], was prepared via the salt-metathesis reaction of N-triisopropyl­silyl-8-amido­quinoline lithium with nickelocene (NiCp2). The asymmetric unit contains two symmetry-independent mol­ecules with the Ni atoms in distorted tetra­hedral environments.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536809051708/jh2120sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536809051708/jh2120Isup2.hkl
Contains datablock I

CCDC reference: 766639

Key indicators

  • Single-crystal X-ray study
  • T = 183 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.047
  • wR factor = 0.123
  • Data-to-parameter ratio = 19.9

checkCIF/PLATON results

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Alert level C PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 5 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 120 PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 5 PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 204
Alert level G PLAT333_ALERT_2_G Check Large Av C6-Ring C-C Dist. C4B -C9B 1.41 Ang. PLAT154_ALERT_1_G The su's on the Cell Angles are Equal (x 10000) 200 Deg. PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 12
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

The reaction of N-trialkylsilyl-8-amidoquinoline lithium (Jonas et al. 2000) with nickelocene yields paramagnetic bis(N-trialkylsilyl-8-amidoquinoline)nickel(II) (Lee et al. 2000) (SiR3 = SiMe3, SiMe2tBu) with the metal centers in distorted tetrahedral environments. Isostructural zinc and magnesium derivatives are thermally stable whereas bis(N-trimethylsilyl-8-amidoquinoline)cadmium(II) liberates dimethylcadmium at 240°C (Englehardt et al. 1991). Transamination of Zn[N(SiMe3)2]2 with N-trialkylsilyl-8-aminoquinoline gives heteroleptic N-trialkylsilyl-8-amidoquinoline zinc(II)bis(trimethylsilyl)amide (Malassa et al. 2008). The metallation of 8-aminoquinoline with [(tmeda)NiMe2] yields bis(8-amidoquinoline) nickel(II) with a square planar coordinated nickel center. In contrast to these rather rare examples of 8-amidoquinoline complexes, neutral 8-aminoquinoline can easily act as a bidentate base to metal cations (see e.g. Engelter et al. 1989, Fanning et al. 1965, Nast et al. 1961, Nielsen et al. 1966).

The reaction of nickelocene with N-triisopropylsilyl-8-amidoquinoline lithium yields the reddish-brown title complex bis(N-triisopropylsilyl-8-amidoquinoline) nickel(II). This compound crystallizes from diethyl ether with two crystallographically independent molecules with similar configurations. The nickel atoms are in distorted tetrahedral environments despite the fact that amido and pyridyl bases have to be considered as strong Lewis bases because the bulky triisopropylsilyl groups prevent a distorted square planar coordination sphere of the Ni centers. Due to an additional electrostatic attraction the Ni—Namido bond lengths (av. value 196.4 pm) are smaller than the Ni—Npyridyl distances with an average value of 200.3 pm.

Related literature top

The reaction of N-trialkylsilyl-8-amidoquinoline lithium (Jonas et al. 2000) with nickelocene yields paramagnetic bis(N-trialkylsilyl-8-amidoquinoline)nickel(II) (Lee et al. 2000). The isostructural zinc and magnesium derivatives are thermally stable whereas bis(N-trimethylsilyl-8-amidoquinoline)cadmium(II) liberates dimethylcadmium at 513 K (Englehardt et al. 1991). Transamination of Zn[N(SiMe3)2]2 with N-trialkylsilyl-8-aminoquinoline gives heteroleptic N-trialkylsilyl-8-amidoquinoline (Malassa et al., 2008). In contrast to these 8-amidoquinoline complexes, neutral 8-aminoquinoline can easily act as a bidentate base to metal cations, see: Engelter et al. (1989); Fanning et al. (1965); Nast et al. (1961); Nielsen & Dahl (1966).

Experimental top

All manipulations were carried out by using modified Schlenk techniques under an atmosphere of argon. Prior to use, THF and diethyl ether were distilled over sodium/benzophenone.

N-Triisopropylsilyl-8-aminochinolin (0.46 g, 1.54 mmol), dissolved at -78°C in 10 ml of THF, was lithiated with 1 mL of a 1,6 M solution of nBuLi in hexane. To this solution 0.15 g of [NiCp2] (1.54 mmol) in 13 ml of THF was added drop-wise while a temperature of -78°C was maintained in the reaction flask. The cooling bath was removed and the red-brown reaction mixture stirred for additional 12 h. Thereafter, all volatiles were removed in vacuum and the residue dissolved in 20 ml of diethyl ether. After filtration the volume of the mother liquor was reduced to half of the original volume. At -20°C reddish brown crystals precipitated. Yield: 0.10 g (0.15 mmol, 21%). IR (Nujol, KBr windows, cm-1): 1562 m,1508 m, 1496 m, 1365 m, 1315 s, 1280 m, 1261 m, 1224 w, 1115 m, 1096 m, 1015 m,934 m, 913 w, 882 m, 819 s, 790 m, 757 m, 739 m, 673 w, 648 w, 621 w, 588 w,561 w, 532 w, 500 w. MS (DEI (%)): m/z = 656 (M+, 5), 614 ([M - iPr]+, 4), 300 (22), 257 (100), 171 (58). Elemental analysis (C36H54N4NiSi2; 657,71 g mol-1): calcd. C 65.74, H 8.28, N 8.52; found C 62.82, H 9.00, N 7.48.

Refinement top

All hydrogen atoms were set to idealized positions and refined with 1.2 times (1.5 for methyl groups) the isotropic displacement parameter of the corresponding carbon atom.

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL/PC (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Molecular structure of I. Displacement ellipsoids are drawn at the 40% probability level. H atoms have been omitted for clarity.
Bis(N-triisopropylsilylquinolin-8-aminato)nickel(II) top
Crystal data top
[Ni(C18H27N2Si)2]Z = 4
Mr = 657.72F(000) = 1416
Triclinic, P1Dx = 1.227 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.3062 (5) ÅCell parameters from 25470 reflections
b = 17.7015 (5) Åθ = 2.0–27.5°
c = 18.4194 (6) ŵ = 0.64 mm1
α = 68.956 (2)°T = 183 K
β = 72.025 (2)°Prism, brown
γ = 85.540 (2)°0.04 × 0.04 × 0.04 mm
V = 3559.6 (2) Å3
Data collection top
Nonius KappaCCD
diffractometer
12031 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.034
Graphite monochromatorθmax = 27.5°, θmin = 2.0°
phi– + ω–scanh = 1514
25470 measured reflectionsk = 2221
15935 independent reflectionsl = 2321
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.047Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.123H-atom parameters constrained
S = 1.02 w = 1/[σ2(Fo2) + (0.0507P)2 + 2.9757P]
where P = (Fo2 + 2Fc2)/3
15935 reflections(Δ/σ)max = 0.001
799 parametersΔρmax = 0.50 e Å3
0 restraintsΔρmin = 0.44 e Å3
Crystal data top
[Ni(C18H27N2Si)2]γ = 85.540 (2)°
Mr = 657.72V = 3559.6 (2) Å3
Triclinic, P1Z = 4
a = 12.3062 (5) ÅMo Kα radiation
b = 17.7015 (5) ŵ = 0.64 mm1
c = 18.4194 (6) ÅT = 183 K
α = 68.956 (2)°0.04 × 0.04 × 0.04 mm
β = 72.025 (2)°
Data collection top
Nonius KappaCCD
diffractometer
12031 reflections with I > 2σ(I)
25470 measured reflectionsRint = 0.034
15935 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0470 restraints
wR(F2) = 0.123H-atom parameters constrained
S = 1.02Δρmax = 0.50 e Å3
15935 reflectionsΔρmin = 0.44 e Å3
799 parameters
Special details top

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 (Å2) top
xyzUiso*/Ueq
Ni1A0.22671 (3)0.404287 (18)0.365455 (19)0.02670 (8)
Si1A0.31556 (6)0.30222 (4)0.52291 (4)0.02685 (15)
Si2A0.28061 (6)0.60410 (4)0.27705 (4)0.02624 (15)
N1A0.06609 (18)0.36971 (12)0.38461 (13)0.0289 (4)
N2A0.20579 (17)0.32527 (12)0.47700 (12)0.0262 (4)
N3A0.30614 (18)0.35165 (12)0.28448 (13)0.0294 (5)
N4A0.30124 (18)0.50415 (12)0.27932 (12)0.0270 (4)
C1A0.0024 (2)0.39528 (16)0.33440 (17)0.0353 (6)
H1AA0.03350.43610.28250.042*
C2A0.1088 (2)0.36428 (18)0.35519 (18)0.0394 (6)
H2AA0.15270.38380.31830.047*
C3A0.1527 (2)0.30520 (17)0.42981 (18)0.0360 (6)
H3AA0.22820.28400.44510.043*
C4A0.0872 (2)0.27538 (15)0.48434 (16)0.0296 (5)
C5A0.1253 (2)0.21290 (16)0.56120 (17)0.0338 (6)
H5AA0.19970.18860.58000.041*
C6A0.0529 (2)0.18804 (16)0.60827 (17)0.0347 (6)
H6AA0.07800.14560.65970.042*
C7A0.0574 (2)0.22324 (15)0.58293 (16)0.0314 (5)
H7AA0.10400.20370.61800.038*
C8A0.1011 (2)0.28572 (14)0.50834 (15)0.0266 (5)
C9A0.0240 (2)0.31006 (14)0.45882 (15)0.0270 (5)
C10A0.3044 (2)0.27422 (16)0.29294 (18)0.0352 (6)
H10A0.25040.23790.33910.042*
C11A0.3797 (2)0.24414 (16)0.23586 (19)0.0378 (6)
H11A0.37720.18820.24360.045*
C12A0.4564 (2)0.29635 (17)0.16916 (18)0.0368 (6)
H12A0.50820.27650.13040.044*
C13A0.4596 (2)0.38015 (16)0.15709 (16)0.0311 (5)
C14A0.5352 (2)0.43815 (17)0.08965 (16)0.0358 (6)
H14A0.58900.42270.04830.043*
C15A0.5295 (2)0.51736 (17)0.08480 (16)0.0365 (6)
H15A0.57980.55680.03900.044*
C16A0.4522 (2)0.54227 (16)0.14508 (16)0.0328 (6)
H16A0.45130.59800.13850.039*
C17A0.3765 (2)0.48775 (15)0.21454 (15)0.0273 (5)
C18A0.3817 (2)0.40518 (15)0.21780 (15)0.0275 (5)
C19A0.3501 (2)0.19049 (15)0.55095 (16)0.0312 (5)
H19A0.28680.16080.60070.037*
C20A0.3507 (3)0.15513 (17)0.48601 (19)0.0406 (7)
H20A0.36580.09720.50530.061*
H20B0.41040.18320.43520.061*
H20C0.27610.16240.47610.061*
C21A0.4609 (2)0.17276 (17)0.57561 (19)0.0396 (6)
H21A0.47320.11440.59220.059*
H21B0.45410.19080.62120.059*
H21C0.52570.20180.52910.059*
C22A0.2903 (2)0.32499 (15)0.62029 (16)0.0330 (6)
H22A0.36710.32090.62910.040*
C23A0.2123 (3)0.2658 (2)0.69940 (18)0.0531 (8)
H23A0.21760.27840.74590.080*
H23B0.23610.21040.70530.080*
H23C0.13310.27090.69770.080*
C24A0.2552 (3)0.41099 (17)0.61376 (18)0.0388 (6)
H24A0.25460.41990.66340.058*
H24B0.17860.41890.60720.058*
H24C0.30980.44960.56640.058*
C25A0.4425 (2)0.37000 (15)0.44380 (16)0.0315 (6)
H25A0.40950.42180.41610.038*
C26A0.5281 (2)0.39364 (18)0.47874 (19)0.0414 (7)
H26A0.58880.42980.43400.062*
H26B0.56180.34470.50810.062*
H26C0.48820.42150.51630.062*
C27A0.5117 (2)0.33914 (18)0.37565 (17)0.0394 (6)
H27A0.56180.38320.33140.059*
H27B0.45940.32020.35450.059*
H27C0.55820.29430.39750.059*
C28A0.1732 (2)0.60344 (15)0.37508 (16)0.0308 (5)
H28A0.16900.66090.37270.037*
C29A0.0512 (2)0.57628 (17)0.38801 (19)0.0397 (6)
H29A0.00010.58310.43760.059*
H29B0.04990.51920.39360.059*
H29C0.02600.60930.34110.059*
C30A0.2114 (3)0.55495 (16)0.45009 (16)0.0363 (6)
H30A0.15770.56230.49870.054*
H30B0.28810.57420.44250.054*
H30C0.21270.49740.45700.054*
C31A0.4195 (2)0.65577 (15)0.26385 (16)0.0329 (6)
H31A0.45480.68280.20370.040*
C32A0.5084 (3)0.59713 (19)0.2939 (2)0.0444 (7)
H32A0.58130.62680.27670.067*
H32B0.51900.55430.27050.067*
H32C0.48160.57290.35350.067*
C33A0.4021 (3)0.72383 (17)0.29984 (19)0.0431 (7)
H33A0.47570.75180.28510.065*
H33B0.37100.70040.35940.065*
H33C0.34870.76250.27790.065*
C34A0.2277 (2)0.66770 (15)0.18740 (16)0.0340 (6)
H34A0.29690.68600.13860.041*
C35A0.1496 (3)0.61987 (18)0.1671 (2)0.0505 (8)
H35A0.13390.65360.11640.076*
H35B0.07760.60450.21160.076*
H35C0.18750.57100.16040.076*
C36A0.1695 (3)0.74443 (17)0.1978 (2)0.0462 (7)
H36A0.14570.77520.14960.069*
H36B0.22320.77780.20430.069*
H36C0.10220.72940.24630.069*
Ni1B0.05709 (3)0.186465 (18)0.17978 (2)0.02737 (9)
Si1B0.21235 (6)0.14247 (4)0.21518 (4)0.02792 (15)
Si2B0.23432 (6)0.11779 (4)0.04677 (4)0.02724 (15)
N1B0.08118 (18)0.30640 (12)0.14648 (13)0.0299 (5)
N2B0.10400 (18)0.21276 (12)0.19249 (13)0.0277 (4)
N3B0.09058 (18)0.14248 (12)0.28678 (13)0.0286 (4)
N4B0.18624 (17)0.12248 (12)0.14461 (13)0.0269 (4)
C1B0.1775 (2)0.34911 (17)0.12183 (17)0.0365 (6)
H1BA0.24670.32120.12130.044*
C2B0.1822 (3)0.43342 (17)0.09647 (18)0.0408 (7)
H2BA0.25310.46220.07890.049*
C3B0.0829 (3)0.47395 (16)0.09732 (18)0.0393 (6)
H3BA0.08500.53150.07840.047*
C4B0.0228 (2)0.43081 (15)0.12615 (16)0.0323 (6)
C5B0.1300 (3)0.46732 (16)0.13364 (19)0.0397 (7)
H5BA0.13480.52450.11800.048*
C6B0.2269 (2)0.41879 (16)0.16390 (19)0.0386 (6)
H6BA0.29910.44320.17050.046*
C7B0.2234 (2)0.33404 (15)0.18565 (18)0.0339 (6)
H7BA0.29320.30310.20690.041*
C8B0.1200 (2)0.29407 (14)0.17684 (15)0.0286 (5)
C9B0.0194 (2)0.34539 (15)0.14931 (15)0.0285 (5)
C10B0.0365 (2)0.15432 (17)0.35555 (17)0.0359 (6)
H10B0.02240.19230.35570.043*
C11B0.0626 (3)0.11292 (17)0.42832 (17)0.0390 (6)
H11B0.02130.12230.47700.047*
C12B0.1483 (3)0.05889 (17)0.42846 (17)0.0382 (6)
H12B0.16640.03020.47760.046*
C13B0.2098 (2)0.04562 (15)0.35589 (16)0.0313 (5)
C14B0.3022 (2)0.00709 (17)0.34931 (18)0.0380 (6)
H14B0.32560.03780.39570.046*
C15B0.3568 (2)0.01270 (17)0.27480 (19)0.0407 (7)
H15B0.42020.04680.27010.049*
C16B0.3239 (2)0.02947 (16)0.20487 (17)0.0335 (6)
H16B0.36570.02330.15470.040*
C17B0.2307 (2)0.08064 (14)0.20711 (15)0.0268 (5)
C18B0.1770 (2)0.08895 (14)0.28493 (15)0.0274 (5)
C19B0.3310 (2)0.13621 (16)0.31244 (17)0.0349 (6)
H19B0.38360.18090.29680.042*
C20B0.2851 (3)0.1516 (2)0.37487 (19)0.0461 (7)
H20D0.34900.15090.42270.069*
H20E0.24450.20450.35000.069*
H20F0.23240.10920.39170.069*
C21B0.4032 (3)0.05698 (18)0.3521 (2)0.0460 (7)
H21D0.46490.05910.40000.069*
H21E0.35490.01140.36900.069*
H21F0.43610.04980.31280.069*
C22B0.2766 (2)0.17488 (17)0.12737 (17)0.0359 (6)
H22B0.30410.23070.12250.043*
C23B0.1873 (3)0.1844 (2)0.04511 (19)0.0522 (8)
H23D0.22280.20710.00130.078*
H23E0.15750.13130.04550.078*
H23F0.12440.22080.03590.078*
C24B0.3821 (3)0.12528 (19)0.1391 (2)0.0438 (7)
H24D0.41190.15050.09260.066*
H24E0.44110.12390.18950.066*
H24F0.36030.06990.14260.066*
C25B0.1370 (2)0.04357 (15)0.22502 (18)0.0364 (6)
H25B0.06180.05850.18130.044*
C26B0.1063 (3)0.00331 (17)0.3047 (2)0.0468 (8)
H26D0.05120.03880.29900.070*
H26E0.17560.02110.34950.070*
H26F0.07260.04410.31670.070*
C27B0.1926 (3)0.02034 (17)0.2077 (2)0.0448 (7)
H27D0.14310.06670.20960.067*
H27E0.20300.00340.15340.067*
H27F0.26700.03840.24890.067*
C28B0.1323 (2)0.18389 (16)0.00721 (17)0.0350 (6)
H28B0.05700.17680.03610.042*
C29B0.1096 (3)0.15814 (19)0.07238 (19)0.0461 (7)
H29D0.05490.19430.09560.069*
H29E0.07800.10240.04760.069*
H29F0.18140.16120.11560.069*
C30B0.1611 (3)0.27536 (17)0.0431 (2)0.0472 (7)
H30D0.09760.30450.06110.071*
H30E0.23060.28700.08980.071*
H30F0.17340.29290.00140.071*
C31B0.2215 (2)0.01270 (16)0.04315 (17)0.0343 (6)
H31B0.22120.02220.01370.041*
C32B0.1061 (3)0.02930 (17)0.0982 (2)0.0460 (7)
H32D0.09880.08010.09000.069*
H32E0.04450.00610.08460.069*
H32F0.10100.04080.15530.069*
C33B0.3175 (3)0.04613 (17)0.0568 (2)0.0453 (7)
H33D0.31050.09090.03900.068*
H33E0.31170.06750.11490.068*
H33F0.39170.01760.02530.068*
C34B0.3898 (2)0.15321 (16)0.00755 (17)0.0345 (6)
H34B0.43610.11040.02060.041*
C35B0.4217 (3)0.23240 (18)0.0014 (2)0.0458 (7)
H35D0.50490.24150.02230.069*
H35E0.39490.22860.05580.069*
H35F0.38560.27770.03380.069*
C36B0.4272 (3)0.15781 (19)0.09643 (18)0.0465 (7)
H36D0.51000.16860.11980.070*
H36E0.38770.20150.12770.070*
H36F0.40770.10620.09870.070*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni1A0.02734 (17)0.02433 (16)0.02715 (16)0.00333 (12)0.00748 (13)0.00737 (12)
Si1A0.0262 (4)0.0254 (3)0.0295 (3)0.0019 (3)0.0103 (3)0.0081 (3)
Si2A0.0282 (4)0.0235 (3)0.0263 (3)0.0022 (3)0.0077 (3)0.0076 (3)
N1A0.0300 (11)0.0262 (10)0.0319 (11)0.0023 (8)0.0117 (9)0.0103 (9)
N2A0.0251 (11)0.0252 (10)0.0274 (10)0.0027 (8)0.0071 (8)0.0080 (8)
N3A0.0294 (11)0.0289 (11)0.0325 (11)0.0006 (8)0.0123 (9)0.0110 (9)
N4A0.0290 (11)0.0246 (10)0.0274 (10)0.0009 (8)0.0085 (9)0.0089 (8)
C1A0.0366 (15)0.0343 (14)0.0360 (14)0.0022 (11)0.0150 (12)0.0103 (11)
C2A0.0346 (15)0.0462 (16)0.0482 (17)0.0080 (12)0.0230 (13)0.0216 (14)
C3A0.0270 (14)0.0411 (15)0.0504 (17)0.0026 (11)0.0139 (12)0.0265 (13)
C4A0.0265 (13)0.0289 (12)0.0378 (14)0.0006 (10)0.0082 (11)0.0180 (11)
C5A0.0251 (13)0.0319 (13)0.0446 (15)0.0025 (10)0.0041 (11)0.0183 (12)
C6A0.0333 (14)0.0293 (13)0.0338 (14)0.0015 (11)0.0022 (11)0.0082 (11)
C7A0.0284 (13)0.0324 (13)0.0305 (13)0.0011 (10)0.0067 (11)0.0095 (11)
C8A0.0250 (12)0.0231 (11)0.0328 (13)0.0006 (9)0.0065 (10)0.0128 (10)
C9A0.0268 (13)0.0248 (12)0.0324 (13)0.0006 (9)0.0081 (10)0.0142 (10)
C10A0.0325 (14)0.0315 (13)0.0447 (15)0.0021 (11)0.0154 (12)0.0132 (12)
C11A0.0338 (15)0.0329 (14)0.0578 (18)0.0034 (11)0.0204 (13)0.0238 (13)
C12A0.0316 (14)0.0428 (15)0.0502 (17)0.0085 (12)0.0191 (13)0.0284 (13)
C13A0.0267 (13)0.0379 (14)0.0361 (14)0.0045 (10)0.0153 (11)0.0174 (11)
C14A0.0292 (14)0.0470 (16)0.0316 (14)0.0048 (12)0.0070 (11)0.0168 (12)
C15A0.0330 (15)0.0429 (15)0.0287 (13)0.0008 (12)0.0056 (11)0.0096 (11)
C16A0.0343 (14)0.0331 (13)0.0305 (13)0.0009 (11)0.0085 (11)0.0111 (11)
C17A0.0266 (13)0.0292 (12)0.0283 (12)0.0002 (10)0.0117 (10)0.0097 (10)
C18A0.0261 (13)0.0313 (12)0.0297 (12)0.0014 (10)0.0141 (10)0.0114 (10)
C19A0.0313 (14)0.0265 (12)0.0363 (14)0.0003 (10)0.0135 (11)0.0088 (10)
C20A0.0475 (17)0.0316 (14)0.0480 (17)0.0018 (12)0.0211 (14)0.0148 (12)
C21A0.0397 (16)0.0329 (14)0.0496 (17)0.0041 (12)0.0222 (13)0.0117 (12)
C22A0.0374 (15)0.0313 (13)0.0334 (14)0.0002 (11)0.0151 (12)0.0110 (11)
C23A0.076 (2)0.0461 (18)0.0320 (15)0.0138 (16)0.0083 (15)0.0115 (13)
C24A0.0406 (16)0.0411 (15)0.0406 (15)0.0058 (12)0.0162 (13)0.0188 (13)
C25A0.0279 (13)0.0294 (13)0.0345 (14)0.0017 (10)0.0104 (11)0.0068 (11)
C26A0.0314 (15)0.0434 (16)0.0510 (17)0.0084 (12)0.0118 (13)0.0171 (14)
C27A0.0302 (14)0.0466 (16)0.0377 (15)0.0037 (12)0.0075 (12)0.0118 (13)
C28A0.0344 (14)0.0246 (12)0.0330 (13)0.0005 (10)0.0077 (11)0.0115 (10)
C29A0.0301 (15)0.0388 (15)0.0458 (16)0.0005 (11)0.0044 (12)0.0155 (13)
C30A0.0430 (16)0.0329 (14)0.0309 (14)0.0004 (11)0.0083 (12)0.0107 (11)
C31A0.0349 (15)0.0330 (13)0.0316 (13)0.0089 (11)0.0091 (11)0.0111 (11)
C32A0.0377 (16)0.0479 (17)0.0546 (18)0.0028 (13)0.0213 (14)0.0191 (14)
C33A0.0496 (18)0.0385 (15)0.0450 (16)0.0133 (13)0.0129 (14)0.0171 (13)
C34A0.0385 (15)0.0292 (13)0.0319 (13)0.0007 (11)0.0120 (12)0.0064 (11)
C35A0.070 (2)0.0395 (16)0.0576 (19)0.0039 (15)0.0422 (18)0.0160 (14)
C36A0.061 (2)0.0297 (14)0.0488 (17)0.0057 (13)0.0256 (15)0.0084 (13)
Ni1B0.02493 (17)0.02550 (16)0.03428 (18)0.00398 (12)0.01139 (13)0.01210 (13)
Si1B0.0247 (3)0.0248 (3)0.0355 (4)0.0003 (3)0.0091 (3)0.0120 (3)
Si2B0.0252 (3)0.0255 (3)0.0302 (3)0.0000 (3)0.0065 (3)0.0104 (3)
N1B0.0271 (11)0.0304 (11)0.0348 (11)0.0010 (8)0.0099 (9)0.0134 (9)
N2B0.0260 (11)0.0243 (10)0.0354 (11)0.0017 (8)0.0102 (9)0.0129 (9)
N3B0.0269 (11)0.0282 (10)0.0327 (11)0.0006 (8)0.0092 (9)0.0125 (9)
N4B0.0235 (10)0.0261 (10)0.0318 (11)0.0029 (8)0.0090 (9)0.0108 (9)
C1B0.0292 (14)0.0394 (15)0.0430 (15)0.0025 (11)0.0101 (12)0.0169 (12)
C2B0.0399 (16)0.0382 (15)0.0449 (16)0.0097 (12)0.0110 (13)0.0148 (13)
C3B0.0484 (18)0.0278 (13)0.0436 (16)0.0072 (12)0.0166 (13)0.0109 (12)
C4B0.0429 (16)0.0247 (12)0.0339 (14)0.0001 (11)0.0171 (12)0.0109 (10)
C5B0.0498 (18)0.0240 (12)0.0529 (17)0.0089 (12)0.0268 (14)0.0142 (12)
C6B0.0356 (15)0.0342 (14)0.0555 (18)0.0123 (11)0.0237 (13)0.0206 (13)
C7B0.0270 (14)0.0310 (13)0.0492 (16)0.0031 (10)0.0159 (12)0.0174 (12)
C8B0.0303 (13)0.0251 (12)0.0335 (13)0.0021 (10)0.0135 (11)0.0110 (10)
C9B0.0303 (13)0.0285 (12)0.0312 (13)0.0014 (10)0.0139 (11)0.0118 (10)
C10B0.0321 (15)0.0383 (14)0.0406 (15)0.0012 (11)0.0086 (12)0.0198 (12)
C11B0.0423 (16)0.0433 (15)0.0340 (14)0.0049 (12)0.0086 (12)0.0178 (12)
C12B0.0437 (17)0.0385 (15)0.0330 (14)0.0084 (12)0.0154 (12)0.0079 (12)
C13B0.0307 (14)0.0300 (13)0.0338 (13)0.0042 (10)0.0129 (11)0.0083 (11)
C14B0.0362 (15)0.0360 (14)0.0412 (16)0.0043 (11)0.0200 (13)0.0066 (12)
C15B0.0316 (15)0.0374 (15)0.0522 (18)0.0095 (12)0.0183 (13)0.0119 (13)
C16B0.0275 (13)0.0349 (14)0.0376 (14)0.0042 (10)0.0094 (11)0.0133 (11)
C17B0.0249 (12)0.0233 (11)0.0334 (13)0.0027 (9)0.0101 (10)0.0096 (10)
C18B0.0255 (12)0.0251 (12)0.0339 (13)0.0033 (9)0.0118 (10)0.0096 (10)
C19B0.0282 (14)0.0347 (14)0.0391 (15)0.0012 (11)0.0058 (11)0.0136 (12)
C20B0.0460 (18)0.0536 (18)0.0423 (17)0.0011 (14)0.0099 (14)0.0241 (14)
C21B0.0375 (16)0.0423 (16)0.0493 (18)0.0074 (13)0.0020 (13)0.0134 (14)
C22B0.0330 (15)0.0350 (14)0.0449 (16)0.0003 (11)0.0170 (12)0.0154 (12)
C23B0.0471 (19)0.070 (2)0.0388 (16)0.0035 (16)0.0153 (14)0.0155 (15)
C24B0.0363 (16)0.0483 (17)0.0584 (19)0.0009 (13)0.0214 (14)0.0261 (15)
C25B0.0306 (14)0.0247 (12)0.0505 (17)0.0005 (10)0.0072 (12)0.0137 (12)
C26B0.0405 (17)0.0289 (14)0.068 (2)0.0029 (12)0.0220 (15)0.0092 (14)
C27B0.0430 (17)0.0291 (14)0.062 (2)0.0000 (12)0.0094 (15)0.0204 (13)
C28B0.0348 (15)0.0376 (14)0.0333 (14)0.0037 (11)0.0116 (11)0.0126 (11)
C29B0.0547 (19)0.0499 (17)0.0411 (16)0.0024 (14)0.0241 (15)0.0166 (14)
C30B0.059 (2)0.0357 (15)0.0495 (18)0.0107 (14)0.0252 (15)0.0118 (13)
C31B0.0318 (14)0.0319 (13)0.0426 (15)0.0007 (11)0.0087 (12)0.0190 (12)
C32B0.0364 (16)0.0350 (15)0.066 (2)0.0039 (12)0.0061 (14)0.0237 (14)
C33B0.0395 (17)0.0351 (15)0.066 (2)0.0051 (12)0.0124 (15)0.0270 (14)
C34B0.0302 (14)0.0318 (13)0.0367 (14)0.0034 (11)0.0048 (11)0.0100 (11)
C35B0.0343 (16)0.0451 (17)0.0565 (19)0.0094 (13)0.0112 (14)0.0162 (14)
C36B0.0413 (17)0.0463 (17)0.0400 (16)0.0031 (13)0.0011 (13)0.0116 (13)
Geometric parameters (Å, º) top
Ni1A—N4A1.955 (2)Ni1B—N4B1.960 (2)
Ni1A—N2A1.977 (2)Ni1B—N2B1.962 (2)
Ni1A—N1A2.002 (2)Ni1B—N3B2.002 (2)
Ni1A—N3A2.001 (2)Ni1B—N1B2.005 (2)
Si1A—N2A1.754 (2)Si1B—N2B1.744 (2)
Si1A—C22A1.906 (3)Si1B—C25B1.892 (3)
Si1A—C19A1.905 (3)Si1B—C22B1.903 (3)
Si1A—C25A1.907 (3)Si1B—C19B1.903 (3)
Si2A—N4A1.755 (2)Si2B—N4B1.745 (2)
Si2A—C28A1.876 (3)Si2B—C34B1.900 (3)
Si2A—C31A1.909 (3)Si2B—C31B1.906 (3)
Si2A—C34A1.906 (3)Si2B—C28B1.908 (3)
N1A—C1A1.328 (3)N1B—C1B1.321 (3)
N1A—C9A1.365 (3)N1B—C9B1.365 (3)
N2A—C8A1.369 (3)N2B—C8B1.374 (3)
N3A—C10A1.324 (3)N3B—C10B1.319 (3)
N3A—C18A1.366 (3)N3B—C18B1.369 (3)
N4A—C17A1.375 (3)N4B—C17B1.373 (3)
C1A—C2A1.401 (4)C1B—C2B1.395 (4)
C1A—H1AA0.9500C1B—H1BA0.9500
C2A—C3A1.368 (4)C2B—C3B1.367 (4)
C2A—H2AA0.9500C2B—H2BA0.9500
C3A—C4A1.411 (4)C3B—C4B1.412 (4)
C3A—H3AA0.9500C3B—H3BA0.9500
C4A—C9A1.413 (4)C4B—C5B1.413 (4)
C4A—C5A1.412 (4)C4B—C9B1.417 (3)
C5A—C6A1.372 (4)C5B—C6B1.369 (4)
C5A—H5AA0.9500C5B—H5BA0.9500
C6A—C7A1.407 (4)C6B—C7B1.408 (4)
C6A—H6AA0.9500C6B—H6BA0.9500
C7A—C8A1.395 (3)C7B—C8B1.400 (4)
C7A—H7AA0.9500C7B—H7BA0.9500
C8A—C9A1.451 (3)C8B—C9B1.440 (4)
C10A—C11A1.404 (4)C10B—C11B1.400 (4)
C10A—H10A0.9500C10B—H10B0.9500
C11A—C12A1.364 (4)C11B—C12B1.367 (4)
C11A—H11A0.9500C11B—H11B0.9500
C12A—C13A1.421 (4)C12B—C13B1.410 (4)
C12A—H12A0.9500C12B—H12B0.9500
C13A—C14A1.408 (4)C13B—C14B1.417 (4)
C13A—C18A1.412 (4)C13B—C18B1.421 (3)
C14A—C15A1.370 (4)C14B—C15B1.365 (4)
C14A—H14A0.9500C14B—H14B0.9500
C15A—C16A1.403 (4)C15B—C16B1.402 (4)
C15A—H15A0.9500C15B—H15B0.9500
C16A—C17A1.398 (4)C16B—C17B1.405 (3)
C16A—H16A0.9500C16B—H16B0.9500
C17A—C18A1.438 (3)C17B—C18B1.437 (4)
C19A—C20A1.534 (4)C19B—C21B1.533 (4)
C19A—C21A1.541 (4)C19B—C20B1.538 (4)
C19A—H19A1.0000C19B—H19B1.0000
C20A—H20A0.9800C20B—H20D0.9800
C20A—H20B0.9800C20B—H20E0.9800
C20A—H20C0.9800C20B—H20F0.9800
C21A—H21A0.9800C21B—H21D0.9800
C21A—H21B0.9800C21B—H21E0.9800
C21A—H21C0.9800C21B—H21F0.9800
C22A—C24A1.522 (4)C22B—C23B1.533 (4)
C22A—C23A1.529 (4)C22B—C24B1.539 (4)
C22A—H22A1.0000C22B—H22B1.0000
C23A—H23A0.9800C23B—H23D0.9800
C23A—H23B0.9800C23B—H23E0.9800
C23A—H23C0.9800C23B—H23F0.9800
C24A—H24A0.9800C24B—H24D0.9800
C24A—H24B0.9800C24B—H24E0.9800
C24A—H24C0.9800C24B—H24F0.9800
C25A—C27A1.536 (4)C25B—C27B1.538 (4)
C25A—C26A1.543 (4)C25B—C26B1.535 (4)
C25A—H25A1.0000C25B—H25B1.0000
C26A—H26A0.9800C26B—H26D0.9800
C26A—H26B0.9800C26B—H26E0.9800
C26A—H26C0.9800C26B—H26F0.9800
C27A—H27A0.9800C27B—H27D0.9800
C27A—H27B0.9800C27B—H27E0.9800
C27A—H27C0.9800C27B—H27F0.9800
C28A—C29A1.533 (4)C28B—C29B1.532 (4)
C28A—C30A1.534 (4)C28B—C30B1.536 (4)
C28A—H28A1.0000C28B—H28B1.0000
C29A—H29A0.9800C29B—H29D0.9800
C29A—H29B0.9800C29B—H29E0.9800
C29A—H29C0.9800C29B—H29F0.9800
C30A—H30A0.9800C30B—H30D0.9800
C30A—H30B0.9800C30B—H30E0.9800
C30A—H30C0.9800C30B—H30F0.9800
C31A—C32A1.538 (4)C31B—C32B1.527 (4)
C31A—C33A1.544 (4)C31B—C33B1.532 (4)
C31A—H31A1.0000C31B—H31B1.0000
C32A—H32A0.9800C32B—H32D0.9800
C32A—H32B0.9800C32B—H32E0.9800
C32A—H32C0.9800C32B—H32F0.9800
C33A—H33A0.9800C33B—H33D0.9800
C33A—H33B0.9800C33B—H33E0.9800
C33A—H33C0.9800C33B—H33F0.9800
C34A—C36A1.532 (4)C34B—C36B1.531 (4)
C34A—C35A1.535 (4)C34B—C35B1.536 (4)
C34A—H34A1.0000C34B—H34B1.0000
C35A—H35A0.9800C35B—H35D0.9800
C35A—H35B0.9800C35B—H35E0.9800
C35A—H35C0.9800C35B—H35F0.9800
C36A—H36A0.9800C36B—H36D0.9800
C36A—H36B0.9800C36B—H36E0.9800
C36A—H36C0.9800C36B—H36F0.9800
N4A—Ni1A—N2A148.45 (9)N4B—Ni1B—N2B148.84 (9)
N4A—Ni1A—N1A122.96 (8)N4B—Ni1B—N3B84.27 (9)
N2A—Ni1A—N1A84.10 (8)N2B—Ni1B—N3B112.36 (9)
N4A—Ni1A—N3A84.62 (9)N4B—Ni1B—N1B118.98 (9)
N2A—Ni1A—N3A109.19 (8)N2B—Ni1B—N1B83.97 (8)
N1A—Ni1A—N3A98.12 (9)N3B—Ni1B—N1B103.14 (8)
N2A—Si1A—C22A116.87 (11)N2B—Si1B—C25B104.23 (11)
N2A—Si1A—C19A111.91 (11)N2B—Si1B—C22B108.52 (11)
C22A—Si1A—C19A105.25 (11)C25B—Si1B—C22B111.75 (13)
N2A—Si1A—C25A104.61 (10)N2B—Si1B—C19B112.00 (12)
C22A—Si1A—C25A106.44 (12)C25B—Si1B—C19B111.95 (12)
C19A—Si1A—C25A111.76 (12)C22B—Si1B—C19B108.35 (13)
N4A—Si2A—C28A109.15 (10)N4B—Si2B—C34B112.65 (11)
N4A—Si2A—C31A111.73 (11)N4B—Si2B—C31B114.47 (11)
C28A—Si2A—C31A108.86 (12)C34B—Si2B—C31B106.42 (12)
N4A—Si2A—C34A110.77 (11)N4B—Si2B—C28B103.96 (11)
C28A—Si2A—C34A109.65 (12)C34B—Si2B—C28B112.80 (12)
C31A—Si2A—C34A106.62 (12)C31B—Si2B—C28B106.53 (12)
C1A—N1A—C9A119.8 (2)C1B—N1B—C9B119.4 (2)
C1A—N1A—Ni1A128.39 (18)C1B—N1B—Ni1B129.09 (18)
C9A—N1A—Ni1A111.79 (16)C9B—N1B—Ni1B111.53 (16)
C8A—N2A—Si1A125.42 (17)C8B—N2B—Si1B124.02 (17)
C8A—N2A—Ni1A111.27 (16)C8B—N2B—Ni1B111.78 (16)
Si1A—N2A—Ni1A122.92 (11)Si1B—N2B—Ni1B124.11 (11)
C10A—N3A—C18A119.9 (2)C10B—N3B—C18B119.7 (2)
C10A—N3A—Ni1A128.79 (19)C10B—N3B—Ni1B128.84 (18)
C18A—N3A—Ni1A110.72 (16)C18B—N3B—Ni1B111.30 (16)
C17A—N4A—Si2A120.87 (16)C17B—N4B—Si2B125.04 (17)
C17A—N4A—Ni1A110.75 (15)C17B—N4B—Ni1B111.40 (16)
Si2A—N4A—Ni1A128.38 (12)Si2B—N4B—Ni1B123.53 (11)
N1A—C1A—C2A122.4 (3)N1B—C1B—C2B122.9 (3)
N1A—C1A—H1AA118.8N1B—C1B—H1BA118.6
C2A—C1A—H1AA118.8C2B—C1B—H1BA118.6
C3A—C2A—C1A118.5 (2)C3B—C2B—C1B118.8 (3)
C3A—C2A—H2AA120.7C3B—C2B—H2BA120.6
C1A—C2A—H2AA120.7C1B—C2B—H2BA120.6
C2A—C3A—C4A120.9 (3)C2B—C3B—C4B120.4 (2)
C2A—C3A—H3AA119.6C2B—C3B—H3BA119.8
C4A—C3A—H3AA119.6C4B—C3B—H3BA119.8
C3A—C4A—C9A117.1 (2)C3B—C4B—C5B124.2 (2)
C3A—C4A—C5A124.1 (2)C3B—C4B—C9B117.0 (2)
C9A—C4A—C5A118.8 (2)C5B—C4B—C9B118.8 (2)
C6A—C5A—C4A118.7 (2)C6B—C5B—C4B118.8 (2)
C6A—C5A—H5AA120.6C6B—C5B—H5BA120.6
C4A—C5A—H5AA120.6C4B—C5B—H5BA120.6
C5A—C6A—C7A122.3 (2)C5B—C6B—C7B122.4 (2)
C5A—C6A—H6AA118.9C5B—C6B—H6BA118.8
C7A—C6A—H6AA118.9C7B—C6B—H6BA118.8
C8A—C7A—C6A122.6 (2)C8B—C7B—C6B121.9 (2)
C8A—C7A—H7AA118.7C8B—C7B—H7BA119.1
C6A—C7A—H7AA118.7C6B—C7B—H7BA119.1
N2A—C8A—C7A128.3 (2)N2B—C8B—C7B128.0 (2)
N2A—C8A—C9A117.4 (2)N2B—C8B—C9B117.0 (2)
C7A—C8A—C9A114.3 (2)C7B—C8B—C9B115.0 (2)
N1A—C9A—C4A121.4 (2)N1B—C9B—C4B121.5 (2)
N1A—C9A—C8A115.3 (2)N1B—C9B—C8B115.6 (2)
C4A—C9A—C8A123.3 (2)C4B—C9B—C8B123.0 (2)
N3A—C10A—C11A122.1 (3)N3B—C10B—C11B122.5 (3)
N3A—C10A—H10A119.0N3B—C10B—H10B118.8
C11A—C10A—H10A119.0C11B—C10B—H10B118.8
C12A—C11A—C10A119.1 (2)C12B—C11B—C10B119.2 (3)
C12A—C11A—H11A120.5C12B—C11B—H11B120.4
C10A—C11A—H11A120.5C10B—C11B—H11B120.4
C11A—C12A—C13A120.6 (3)C11B—C12B—C13B120.2 (3)
C11A—C12A—H12A119.7C11B—C12B—H12B119.9
C13A—C12A—H12A119.7C13B—C12B—H12B119.9
C14A—C13A—C18A119.1 (2)C12B—C13B—C14B124.3 (2)
C14A—C13A—C12A124.2 (3)C12B—C13B—C18B117.2 (2)
C18A—C13A—C12A116.7 (2)C14B—C13B—C18B118.4 (2)
C15A—C14A—C13A118.6 (3)C15B—C14B—C13B118.5 (2)
C15A—C14A—H14A120.7C15B—C14B—H14B120.7
C13A—C14A—H14A120.7C13B—C14B—H14B120.7
C14A—C15A—C16A122.3 (3)C14B—C15B—C16B123.1 (3)
C14A—C15A—H15A118.9C14B—C15B—H15B118.4
C16A—C15A—H15A118.9C16B—C15B—H15B118.4
C17A—C16A—C15A122.2 (2)C15B—C16B—C17B121.7 (3)
C17A—C16A—H16A118.9C15B—C16B—H16B119.1
C15A—C16A—H16A118.9C17B—C16B—H16B119.1
N4A—C17A—C16A127.5 (2)N4B—C17B—C16B127.8 (2)
N4A—C17A—C18A117.7 (2)N4B—C17B—C18B117.5 (2)
C16A—C17A—C18A114.8 (2)C16B—C17B—C18B114.7 (2)
N3A—C18A—C13A121.7 (2)N3B—C18B—C13B121.2 (2)
N3A—C18A—C17A115.4 (2)N3B—C18B—C17B115.3 (2)
C13A—C18A—C17A122.9 (2)C13B—C18B—C17B123.4 (2)
C20A—C19A—C21A111.7 (2)C21B—C19B—C20B110.4 (2)
C20A—C19A—Si1A113.78 (18)C21B—C19B—Si1B113.8 (2)
C21A—C19A—Si1A112.23 (18)C20B—C19B—Si1B111.94 (19)
C20A—C19A—H19A106.2C21B—C19B—H19B106.8
C21A—C19A—H19A106.2C20B—C19B—H19B106.8
Si1A—C19A—H19A106.2Si1B—C19B—H19B106.8
C19A—C20A—H20A109.5C19B—C20B—H20D109.5
C19A—C20A—H20B109.5C19B—C20B—H20E109.5
H20A—C20A—H20B109.5H20D—C20B—H20E109.5
C19A—C20A—H20C109.5C19B—C20B—H20F109.5
H20A—C20A—H20C109.5H20D—C20B—H20F109.5
H20B—C20A—H20C109.5H20E—C20B—H20F109.5
C19A—C21A—H21A109.5C19B—C21B—H21D109.5
C19A—C21A—H21B109.5C19B—C21B—H21E109.5
H21A—C21A—H21B109.5H21D—C21B—H21E109.5
C19A—C21A—H21C109.5C19B—C21B—H21F109.5
H21A—C21A—H21C109.5H21D—C21B—H21F109.5
H21B—C21A—H21C109.5H21E—C21B—H21F109.5
C24A—C22A—C23A108.8 (2)C23B—C22B—C24B110.4 (2)
C24A—C22A—Si1A114.80 (18)C23B—C22B—Si1B112.7 (2)
C23A—C22A—Si1A117.6 (2)C24B—C22B—Si1B116.8 (2)
C24A—C22A—H22A104.8C23B—C22B—H22B105.3
C23A—C22A—H22A104.8C24B—C22B—H22B105.3
Si1A—C22A—H22A104.8Si1B—C22B—H22B105.3
C22A—C23A—H23A109.5C22B—C23B—H23D109.5
C22A—C23A—H23B109.5C22B—C23B—H23E109.5
H23A—C23A—H23B109.5H23D—C23B—H23E109.5
C22A—C23A—H23C109.5C22B—C23B—H23F109.5
H23A—C23A—H23C109.5H23D—C23B—H23F109.5
H23B—C23A—H23C109.5H23E—C23B—H23F109.5
C22A—C24A—H24A109.5C22B—C24B—H24D109.5
C22A—C24A—H24B109.5C22B—C24B—H24E109.5
H24A—C24A—H24B109.5H24D—C24B—H24E109.5
C22A—C24A—H24C109.5C22B—C24B—H24F109.5
H24A—C24A—H24C109.5H24D—C24B—H24F109.5
H24B—C24A—H24C109.5H24E—C24B—H24F109.5
C27A—C25A—C26A107.4 (2)C27B—C25B—C26B109.3 (2)
C27A—C25A—Si1A115.79 (18)C27B—C25B—Si1B116.5 (2)
C26A—C25A—Si1A115.25 (19)C26B—C25B—Si1B115.1 (2)
C27A—C25A—H25A105.8C27B—C25B—H25B104.9
C26A—C25A—H25A105.8C26B—C25B—H25B104.9
Si1A—C25A—H25A105.8Si1B—C25B—H25B104.9
C25A—C26A—H26A109.5C25B—C26B—H26D109.5
C25A—C26A—H26B109.5C25B—C26B—H26E109.5
H26A—C26A—H26B109.5H26D—C26B—H26E109.5
C25A—C26A—H26C109.5C25B—C26B—H26F109.5
H26A—C26A—H26C109.5H26D—C26B—H26F109.5
H26B—C26A—H26C109.5H26E—C26B—H26F109.5
C25A—C27A—H27A109.5C25B—C27B—H27D109.5
C25A—C27A—H27B109.5C25B—C27B—H27E109.5
H27A—C27A—H27B109.5H27D—C27B—H27E109.5
C25A—C27A—H27C109.5C25B—C27B—H27F109.5
H27A—C27A—H27C109.5H27D—C27B—H27F109.5
H27B—C27A—H27C109.5H27E—C27B—H27F109.5
C29A—C28A—C30A109.8 (2)C29B—C28B—C30B108.7 (2)
C29A—C28A—Si2A115.17 (19)C29B—C28B—Si2B115.1 (2)
C30A—C28A—Si2A112.65 (18)C30B—C28B—Si2B115.7 (2)
C29A—C28A—H28A106.2C29B—C28B—H28B105.4
C30A—C28A—H28A106.2C30B—C28B—H28B105.4
Si2A—C28A—H28A106.2Si2B—C28B—H28B105.4
C28A—C29A—H29A109.5C28B—C29B—H29D109.5
C28A—C29A—H29B109.5C28B—C29B—H29E109.5
H29A—C29A—H29B109.5H29D—C29B—H29E109.5
C28A—C29A—H29C109.5C28B—C29B—H29F109.5
H29A—C29A—H29C109.5H29D—C29B—H29F109.5
H29B—C29A—H29C109.5H29E—C29B—H29F109.5
C28A—C30A—H30A109.5C28B—C30B—H30D109.5
C28A—C30A—H30B109.5C28B—C30B—H30E109.5
H30A—C30A—H30B109.5H30D—C30B—H30E109.5
C28A—C30A—H30C109.5C28B—C30B—H30F109.5
H30A—C30A—H30C109.5H30D—C30B—H30F109.5
H30B—C30A—H30C109.5H30E—C30B—H30F109.5
C32A—C31A—C33A110.2 (2)C32B—C31B—C33B109.7 (2)
C32A—C31A—Si2A114.30 (18)C32B—C31B—Si2B111.68 (19)
C33A—C31A—Si2A114.0 (2)C33B—C31B—Si2B118.6 (2)
C32A—C31A—H31A105.9C32B—C31B—H31B105.3
C33A—C31A—H31A105.9C33B—C31B—H31B105.3
Si2A—C31A—H31A105.9Si2B—C31B—H31B105.3
C31A—C32A—H32A109.5C31B—C32B—H32D109.5
C31A—C32A—H32B109.5C31B—C32B—H32E109.5
H32A—C32A—H32B109.5H32D—C32B—H32E109.5
C31A—C32A—H32C109.5C31B—C32B—H32F109.5
H32A—C32A—H32C109.5H32D—C32B—H32F109.5
H32B—C32A—H32C109.5H32E—C32B—H32F109.5
C31A—C33A—H33A109.5C31B—C33B—H33D109.5
C31A—C33A—H33B109.5C31B—C33B—H33E109.5
H33A—C33A—H33B109.5H33D—C33B—H33E109.5
C31A—C33A—H33C109.5C31B—C33B—H33F109.5
H33A—C33A—H33C109.5H33D—C33B—H33F109.5
H33B—C33A—H33C109.5H33E—C33B—H33F109.5
C36A—C34A—C35A109.9 (2)C36B—C34B—C35B111.0 (2)
C36A—C34A—Si2A113.1 (2)C36B—C34B—Si2B112.1 (2)
C35A—C34A—Si2A113.44 (18)C35B—C34B—Si2B114.5 (2)
C36A—C34A—H34A106.6C36B—C34B—H34B106.2
C35A—C34A—H34A106.6C35B—C34B—H34B106.2
Si2A—C34A—H34A106.6Si2B—C34B—H34B106.2
C34A—C35A—H35A109.5C34B—C35B—H35D109.5
C34A—C35A—H35B109.5C34B—C35B—H35E109.5
H35A—C35A—H35B109.5H35D—C35B—H35E109.5
C34A—C35A—H35C109.5C34B—C35B—H35F109.5
H35A—C35A—H35C109.5H35D—C35B—H35F109.5
H35B—C35A—H35C109.5H35E—C35B—H35F109.5
C34A—C36A—H36A109.5C34B—C36B—H36D109.5
C34A—C36A—H36B109.5C34B—C36B—H36E109.5
H36A—C36A—H36B109.5H36D—C36B—H36E109.5
C34A—C36A—H36C109.5C34B—C36B—H36F109.5
H36A—C36A—H36C109.5H36D—C36B—H36F109.5
H36B—C36A—H36C109.5H36E—C36B—H36F109.5

Experimental details

Crystal data
Chemical formula[Ni(C18H27N2Si)2]
Mr657.72
Crystal system, space groupTriclinic, P1
Temperature (K)183
a, b, c (Å)12.3062 (5), 17.7015 (5), 18.4194 (6)
α, β, γ (°)68.956 (2), 72.025 (2), 85.540 (2)
V3)3559.6 (2)
Z4
Radiation typeMo Kα
µ (mm1)0.64
Crystal size (mm)0.04 × 0.04 × 0.04
Data collection
DiffractometerNonius KappaCCD
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
25470, 15935, 12031
Rint0.034
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.047, 0.123, 1.02
No. of reflections15935
No. of parameters799
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.50, 0.44

Computer programs: COLLECT (Nonius, 1998), DENZO (Otwinowski & Minor, 1997), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL/PC (Sheldrick, 2008).

 

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