Download citation
Download citation
link to html
The title tetra­nuclear nickel(II) compound, [Ni4(C15H16N2O2)4], is isostructural with the zinc(II) complex reported recently [You, Ma, Zhu & Liu (2004). Acta Cryst. E60, m1599-m1601]. The complex has {\overline 4} crystallographic symmetry. Each NiII atom has a distorted square-pyramidal geometry. In the basal plane, the Ni atom is coordinated by two N atoms and two O atoms of a Schiff base. The apical position is occupied by another O atom of another Schiff base.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805017058/br6196sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805017058/br6196Isup2.hkl
Contains datablock I

CCDC reference: 267822

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.049
  • wR factor = 0.123
  • Data-to-parameter ratio = 15.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 PLAT731_ALERT_1_C Bond Calc 0.89(3), Rep 0.892(10) ...... 3.00 su-Rat N2 -H2 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

cyclo-Tetrakis{µ-1-[2-(2-oxidoethylamino)ethyliminomethyl]naphthalen-2- olato}tetranickel(II) top
Crystal data top
[Ni4(C15H16N2O2)4]Dx = 1.481 Mg m3
Mr = 1260.03Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P42/nCell parameters from 1898 reflections
Hall symbol: -P 4bcθ = 2.1–22.4°
a = 18.1814 (8) ŵ = 1.38 mm1
c = 8.5460 (7) ÅT = 298 K
V = 2825.0 (3) Å3Block, green
Z = 20.34 × 0.28 × 0.22 mm
F(000) = 1312
Data collection top
Bruker SMART CCD area-detector
diffractometer
2917 independent reflections
Radiation source: fine-focus sealed tube2333 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.041
ω scansθmax = 26.5°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 2219
Tmin = 0.652, Tmax = 0.752k = 2222
12894 measured reflectionsl = 710
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)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.123H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + (0.0637P)2 + 1.4827P]
where P = (Fo2 + 2Fc2)/3
2917 reflections(Δ/σ)max < 0.001
184 parametersΔρmax = 0.40 e Å3
1 restraintΔρmin = 0.38 e Å3
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
Ni10.80929 (2)0.62242 (2)0.22739 (5)0.03188 (16)
O10.76479 (11)0.58192 (11)0.0287 (3)0.0358 (5)
O20.71257 (11)0.63713 (12)0.3366 (2)0.0338 (5)
N10.87882 (14)0.53371 (14)0.2209 (3)0.0349 (6)
N20.84955 (14)0.62482 (13)0.4668 (3)0.0330 (6)
C10.84331 (15)0.47916 (16)0.0281 (4)0.0299 (6)
C20.78005 (16)0.52376 (16)0.0515 (4)0.0305 (6)
C30.72853 (18)0.50169 (18)0.1686 (4)0.0379 (7)
H30.68670.53010.18450.045*
C40.7384 (2)0.44118 (19)0.2568 (4)0.0427 (8)
H40.70200.42730.32720.051*
C50.8033 (2)0.39821 (18)0.2444 (4)0.0402 (8)
C60.8140 (2)0.3371 (2)0.3437 (5)0.0583 (10)
H60.77770.32410.41520.070*
C70.8769 (3)0.2970 (2)0.3356 (6)0.0718 (13)
H70.88350.25650.40060.086*
C80.9313 (3)0.3166 (3)0.2304 (5)0.0664 (12)
H80.97450.28940.22640.080*
C90.9225 (2)0.3756 (2)0.1317 (4)0.0480 (9)
H90.96020.38790.06300.058*
C100.85714 (17)0.41797 (16)0.1327 (4)0.0331 (7)
C110.88714 (17)0.48664 (16)0.1097 (4)0.0355 (7)
H110.92610.45380.12030.043*
C120.92493 (18)0.5275 (2)0.3612 (4)0.0438 (8)
H12A0.96820.55830.35080.053*
H12B0.94080.47690.37510.053*
C130.87991 (18)0.55172 (18)0.4995 (4)0.0396 (8)
H13A0.84030.51700.51800.048*
H13B0.91050.55350.59240.048*
C140.78796 (18)0.64689 (18)0.5671 (4)0.0379 (7)
H14A0.78610.70010.57490.046*
H14B0.79460.62690.67140.046*
C150.71712 (17)0.61839 (19)0.4975 (4)0.0370 (7)
H15A0.71500.56540.50910.044*
H15B0.67560.63940.55320.044*
H20.8859 (16)0.6576 (18)0.473 (5)0.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0316 (2)0.0280 (2)0.0361 (3)0.00098 (16)0.00211 (17)0.00299 (16)
O10.0372 (11)0.0299 (11)0.0404 (12)0.0099 (9)0.0083 (10)0.0060 (10)
O20.0284 (11)0.0425 (12)0.0306 (11)0.0055 (9)0.0006 (9)0.0054 (10)
N10.0284 (13)0.0343 (14)0.0419 (15)0.0055 (11)0.0051 (12)0.0018 (12)
N20.0293 (13)0.0301 (14)0.0396 (15)0.0050 (11)0.0068 (12)0.0028 (11)
C10.0261 (14)0.0286 (15)0.0350 (16)0.0006 (12)0.0056 (12)0.0057 (13)
C20.0307 (15)0.0290 (15)0.0319 (16)0.0012 (13)0.0043 (13)0.0042 (13)
C30.0362 (17)0.0368 (17)0.0407 (18)0.0098 (14)0.0027 (14)0.0002 (15)
C40.0433 (19)0.0431 (19)0.042 (2)0.0001 (16)0.0046 (15)0.0063 (15)
C50.048 (2)0.0328 (17)0.0400 (19)0.0049 (15)0.0111 (15)0.0020 (14)
C60.065 (3)0.051 (2)0.059 (2)0.006 (2)0.005 (2)0.021 (2)
C70.086 (3)0.061 (3)0.069 (3)0.023 (2)0.014 (3)0.028 (2)
C80.066 (3)0.066 (3)0.067 (3)0.034 (2)0.015 (2)0.007 (2)
C90.045 (2)0.049 (2)0.049 (2)0.0142 (17)0.0096 (17)0.0014 (17)
C100.0352 (16)0.0280 (15)0.0359 (17)0.0032 (12)0.0124 (14)0.0054 (13)
C110.0294 (16)0.0306 (16)0.0465 (18)0.0051 (13)0.0030 (14)0.0059 (14)
C120.0348 (17)0.048 (2)0.048 (2)0.0075 (15)0.0117 (15)0.0016 (16)
C130.0386 (18)0.0393 (18)0.0409 (18)0.0014 (14)0.0112 (15)0.0101 (15)
C140.0453 (19)0.0356 (17)0.0328 (17)0.0014 (14)0.0033 (14)0.0018 (14)
C150.0359 (17)0.0456 (18)0.0295 (16)0.0017 (14)0.0001 (13)0.0078 (14)
Geometric parameters (Å, º) top
Ni1—O2i1.984 (2)C5—C61.412 (5)
Ni1—O22.009 (2)C5—C101.414 (5)
Ni1—O12.020 (2)C6—C71.358 (6)
Ni1—N12.050 (3)C6—H60.9300
Ni1—N22.174 (3)C7—C81.382 (7)
O1—C21.290 (3)C7—H70.9300
O2—C151.419 (4)C8—C91.374 (6)
O2—Ni1ii1.984 (2)C8—H80.9300
N1—C111.288 (4)C9—C101.417 (4)
N1—C121.467 (4)C9—H90.9300
N2—C141.466 (4)C11—H110.9300
N2—C131.466 (4)C12—C131.504 (5)
N2—H20.892 (10)C12—H12A0.9700
C1—C21.421 (4)C12—H12B0.9700
C1—C111.428 (4)C13—H13A0.9700
C1—C101.449 (4)C13—H13B0.9700
C2—C31.428 (4)C14—C151.510 (4)
C3—C41.346 (5)C14—H14A0.9700
C3—H30.9300C14—H14B0.9700
C4—C51.418 (5)C15—H15A0.9700
C4—H40.9300C15—H15B0.9700
O2i—Ni1—O2116.62 (12)C5—C6—H6119.7
O2i—Ni1—O1105.45 (9)C6—C7—C8119.8 (4)
O2—Ni1—O195.07 (9)C6—C7—H7120.1
O2i—Ni1—N1109.87 (10)C8—C7—H7120.1
O2—Ni1—N1131.08 (10)C9—C8—C7121.2 (4)
O1—Ni1—N186.42 (9)C9—C8—H8119.4
O2i—Ni1—N294.45 (9)C7—C8—H8119.4
O2—Ni1—N281.65 (9)C8—C9—C10121.2 (4)
O1—Ni1—N2158.99 (9)C8—C9—H9119.4
N1—Ni1—N280.41 (10)C10—C9—H9119.4
C2—O1—Ni1131.24 (19)C5—C10—C9116.6 (3)
C15—O2—Ni1ii115.67 (18)C5—C10—C1119.4 (3)
C15—O2—Ni1111.54 (17)C9—C10—C1124.0 (3)
Ni1ii—O2—Ni1131.35 (11)N1—C11—C1127.3 (3)
C11—N1—C12119.0 (3)N1—C11—H11116.3
C11—N1—Ni1128.0 (2)C1—C11—H11116.3
C12—N1—Ni1113.0 (2)N1—C12—C13108.0 (3)
C14—N2—C13115.1 (3)N1—C12—H12A110.1
C14—N2—Ni1107.37 (18)C13—C12—H12A110.1
C13—N2—Ni1106.74 (19)N1—C12—H12B110.1
C14—N2—H2110 (3)C13—C12—H12B110.1
C13—N2—H2108 (3)H12A—C12—H12B108.4
Ni1—N2—H2109 (3)N2—C13—C12108.7 (3)
C2—C1—C11120.9 (3)N2—C13—H13A109.9
C2—C1—C10119.4 (3)C12—C13—H13A109.9
C11—C1—C10119.0 (3)N2—C13—H13B109.9
O1—C2—C1124.5 (3)C12—C13—H13B109.9
O1—C2—C3117.5 (3)H13A—C13—H13B108.3
C1—C2—C3118.0 (3)N2—C14—C15109.1 (3)
C4—C3—C2122.3 (3)N2—C14—H14A109.9
C4—C3—H3118.8C15—C14—H14A109.9
C2—C3—H3118.8N2—C14—H14B109.9
C3—C4—C5121.3 (3)C15—C14—H14B109.9
C3—C4—H4119.3H14A—C14—H14B108.3
C5—C4—H4119.3O2—C15—C14110.4 (3)
C6—C5—C10120.7 (3)O2—C15—H15A109.6
C6—C5—C4120.3 (3)C14—C15—H15A109.6
C10—C5—C4119.1 (3)O2—C15—H15B109.6
C7—C6—C5120.5 (4)C14—C15—H15B109.6
C7—C6—H6119.7H15A—C15—H15B108.1
Symmetry codes: (i) y+3/2, x, z+1/2; (ii) y, x+3/2, z+1/2.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds