Download citation
Download citation
link to html
In the title complex, [Ni(C15H13N5)2](NO3)2, the NiII ion is located on a twofold axis and is chelated by two tridentate 2,6-bis­(2-pyridylamino)pyridine ligands in an octa­hedral geometry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806049919/ww2052sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806049919/ww2052Isup2.hkl
Contains datablock I

CCDC reference: 630509

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • R factor = 0.051
  • wR factor = 0.148
  • Data-to-parameter ratio = 12.4

checkCIF/PLATON results

No syntax errors found


No errors found in this datablock

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2; data reduction: APEX2; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
[Ni(C15H13N5)2](NO3)2F(000) = 732
Mr = 709.34Dx = 1.520 Mg m3
Monoclinic, P2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ycCell parameters from 2003 reflections
a = 8.2138 (12) Åθ = 2.4–23.9°
b = 11.2601 (16) ŵ = 0.69 mm1
c = 16.790 (2) ÅT = 296 K
β = 93.277 (2)°Block, green
V = 1550.4 (4) Å30.35 × 0.14 × 0.13 mm
Z = 2
Data collection top
Bruker APEX-II area-detector
diffractometer
2759 independent reflections
Radiation source: fine-focus sealed tube2318 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
φ and ω scansθmax = 25.1°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 99
Tmin = 0.795, Tmax = 0.918k = 1311
7719 measured reflectionsl = 2017
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)] = 0.051Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.148H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.0783P)2 + 1.716P]
where P = (Fo2 + 2Fc2)/3
2759 reflections(Δ/σ)max < 0.001
222 parametersΔρmax = 0.93 e Å3
0 restraintsΔρmin = 0.73 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 > 2σ(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
Ni10.00000.26925 (5)0.25000.0351 (2)
N10.1211 (3)0.3997 (2)0.18149 (16)0.0398 (6)
N20.1259 (4)0.4716 (2)0.13687 (18)0.0478 (7)
H2A0.18380.53520.13630.057*
N30.1751 (3)0.2682 (2)0.16589 (16)0.0385 (6)
N40.2278 (4)0.0648 (2)0.19245 (17)0.0498 (7)
H4A0.22030.00080.16450.060*
N50.1403 (3)0.1421 (2)0.31250 (16)0.0414 (6)
N60.2921 (4)0.7693 (3)0.1099 (2)0.0597 (9)
O10.3013 (4)0.6746 (3)0.0771 (2)0.0845 (11)
O20.3893 (5)0.8475 (3)0.1143 (3)0.1027 (13)
C10.2837 (4)0.4150 (3)0.1863 (2)0.0466 (8)
H10.34490.35110.20280.056*
C20.3627 (5)0.5188 (3)0.1683 (2)0.0527 (9)
H20.47470.52560.17260.063*
C30.2713 (5)0.6139 (3)0.1434 (3)0.0603 (10)
H30.32050.68720.13350.072*
C40.1097 (5)0.5992 (3)0.1336 (3)0.0585 (10)
H40.04760.66180.11570.070*
C50.0371 (4)0.4883 (3)0.15088 (19)0.0420 (8)
C60.2090 (4)0.3668 (3)0.12362 (19)0.0415 (8)
C70.3278 (5)0.3682 (3)0.0680 (2)0.0516 (9)
H70.34890.43730.04010.062*
C80.4134 (5)0.2666 (4)0.0549 (2)0.0593 (10)
H80.49400.26640.01820.071*
C90.3800 (5)0.1646 (4)0.0961 (2)0.0546 (9)
H90.43620.09470.08700.065*
C100.2608 (4)0.1678 (3)0.15166 (19)0.0425 (8)
C110.2054 (4)0.0527 (3)0.2733 (2)0.0451 (8)
C120.2541 (6)0.0521 (3)0.3124 (3)0.0653 (11)
H120.29490.11540.28390.078*
C130.2410 (6)0.0603 (4)0.3924 (3)0.0715 (13)
H130.27090.13000.41900.086*
C140.1832 (5)0.0353 (3)0.4342 (2)0.0560 (9)
H140.17830.03250.48940.067*
C150.1341 (4)0.1327 (3)0.3926 (2)0.0475 (8)
H150.09400.19680.42040.057*
O30.1554 (7)0.8087 (6)0.1204 (5)0.203 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0408 (4)0.0269 (3)0.0384 (3)0.0000.0086 (2)0.000
N10.0429 (15)0.0307 (14)0.0462 (16)0.0027 (11)0.0045 (12)0.0018 (11)
N20.0498 (17)0.0334 (15)0.0613 (19)0.0067 (12)0.0124 (13)0.0049 (13)
N30.0445 (15)0.0322 (14)0.0393 (15)0.0017 (11)0.0086 (12)0.0016 (11)
N40.072 (2)0.0317 (15)0.0468 (17)0.0080 (14)0.0137 (14)0.0059 (12)
N50.0510 (16)0.0335 (14)0.0402 (15)0.0053 (12)0.0060 (12)0.0004 (11)
N60.056 (2)0.051 (2)0.074 (2)0.0079 (16)0.0266 (17)0.0100 (17)
O10.109 (3)0.0404 (16)0.110 (3)0.0135 (16)0.059 (2)0.0121 (17)
O20.104 (3)0.072 (2)0.136 (3)0.029 (2)0.040 (2)0.024 (2)
C10.0461 (19)0.0416 (19)0.052 (2)0.0036 (15)0.0031 (15)0.0068 (16)
C20.049 (2)0.051 (2)0.058 (2)0.0072 (17)0.0007 (16)0.0044 (17)
C30.060 (2)0.040 (2)0.080 (3)0.0113 (17)0.000 (2)0.0098 (19)
C40.069 (3)0.0359 (19)0.071 (3)0.0038 (17)0.005 (2)0.0136 (18)
C50.0493 (19)0.0357 (17)0.0411 (18)0.0034 (14)0.0032 (14)0.0022 (14)
C60.0443 (18)0.0394 (18)0.0415 (18)0.0082 (14)0.0082 (14)0.0006 (14)
C70.055 (2)0.053 (2)0.048 (2)0.0117 (17)0.0153 (17)0.0005 (16)
C80.056 (2)0.074 (3)0.050 (2)0.006 (2)0.0227 (18)0.0085 (19)
C90.053 (2)0.055 (2)0.057 (2)0.0041 (17)0.0151 (17)0.0135 (18)
C100.0464 (18)0.0420 (19)0.0398 (17)0.0020 (15)0.0072 (14)0.0082 (14)
C110.052 (2)0.0346 (18)0.0492 (19)0.0032 (14)0.0046 (15)0.0025 (14)
C120.097 (3)0.039 (2)0.061 (3)0.022 (2)0.008 (2)0.0023 (18)
C130.106 (4)0.045 (2)0.064 (3)0.020 (2)0.003 (2)0.0136 (19)
C140.072 (3)0.050 (2)0.045 (2)0.0065 (19)0.0007 (17)0.0066 (17)
C150.054 (2)0.0426 (19)0.046 (2)0.0042 (15)0.0051 (15)0.0002 (15)
O30.114 (4)0.147 (5)0.356 (11)0.030 (4)0.093 (5)0.117 (6)
Geometric parameters (Å, º) top
Ni1—N32.073 (3)C1—H10.9300
Ni1—N3i2.073 (3)C2—C31.386 (5)
Ni1—N5i2.083 (3)C2—H20.9300
Ni1—N52.083 (3)C3—C41.357 (6)
Ni1—N1i2.083 (3)C3—H30.9300
Ni1—N12.083 (3)C4—C51.407 (5)
N1—C51.333 (4)C4—H40.9300
N1—C11.354 (4)C6—C71.389 (5)
N2—C51.385 (4)C7—C81.366 (5)
N2—C61.388 (4)C7—H70.9300
N2—H2A0.8600C8—C91.377 (6)
N3—C61.355 (4)C8—H80.9300
N3—C101.359 (4)C9—C101.390 (5)
N4—C101.382 (4)C9—H90.9300
N4—C111.388 (4)C11—C121.398 (5)
N4—H4A0.8600C12—C131.356 (6)
N5—C111.331 (4)C12—H120.9300
N5—C151.353 (4)C13—C141.385 (6)
N6—O21.188 (4)C13—H130.9300
N6—O11.204 (4)C14—C151.350 (5)
N6—O31.230 (6)C14—H140.9300
C1—C21.362 (5)C15—H150.9300
N3—Ni1—N3i179.33 (14)C4—C3—C2119.6 (3)
N3—Ni1—N5i92.18 (11)C4—C3—H3120.2
N3i—Ni1—N5i87.35 (11)C2—C3—H3120.2
N3—Ni1—N587.35 (11)C3—C4—C5119.3 (3)
N3i—Ni1—N592.18 (10)C3—C4—H4120.4
N5i—Ni1—N593.18 (15)C5—C4—H4120.4
N3—Ni1—N1i93.00 (10)N1—C5—N2119.4 (3)
N3i—Ni1—N1i87.47 (10)N1—C5—C4121.4 (3)
N5i—Ni1—N1i174.62 (10)N2—C5—C4119.2 (3)
N5—Ni1—N1i88.50 (11)N3—C6—N2119.7 (3)
N3—Ni1—N187.47 (10)N3—C6—C7122.3 (3)
N3i—Ni1—N193.00 (10)N2—C6—C7118.0 (3)
N5i—Ni1—N188.50 (11)C8—C7—C6119.1 (3)
N5—Ni1—N1174.62 (10)C8—C7—H7120.4
N1—Ni1—N1i90.30 (15)C6—C7—H7120.4
C5—N1—C1117.5 (3)C7—C8—C9119.8 (3)
C5—N1—Ni1120.0 (2)C7—C8—H8120.1
C1—N1—Ni1119.9 (2)C9—C8—H8120.1
C5—N2—C6129.2 (3)C8—C9—C10118.9 (3)
C5—N2—H2A115.4C8—C9—H9120.5
C6—N2—H2A115.4C10—C9—H9120.5
C6—N3—C10117.7 (3)N3—C10—N4119.5 (3)
C6—N3—Ni1121.6 (2)N3—C10—C9122.1 (3)
C10—N3—Ni1120.7 (2)N4—C10—C9118.4 (3)
C10—N4—C11127.4 (3)N5—C11—N4119.3 (3)
C10—N4—H4A116.3N5—C11—C12121.3 (3)
C11—N4—H4A116.3N4—C11—C12119.4 (3)
C11—N5—C15118.1 (3)C13—C12—C11119.0 (4)
C11—N5—Ni1119.8 (2)C13—C12—H12120.5
C15—N5—Ni1120.2 (2)C11—C12—H12120.5
O2—N6—O1128.7 (4)C12—C13—C14119.9 (4)
O2—N6—O3109.9 (4)C12—C13—H13120.0
O1—N6—O3117.8 (4)C14—C13—H13120.0
N1—C1—C2123.7 (3)C15—C14—C13118.0 (4)
N1—C1—H1118.1C15—C14—H14121.0
C2—C1—H1118.1C13—C14—H14121.0
C1—C2—C3118.0 (4)C14—C15—N5123.5 (3)
C1—C2—H2121.0C14—C15—H15118.3
C3—C2—H2121.0N5—C15—H15118.3
N3—Ni1—N1—C543.2 (2)C1—N1—C5—C48.0 (5)
N3i—Ni1—N1—C5137.3 (2)Ni1—N1—C5—C4153.7 (3)
N5i—Ni1—N1—C5135.4 (3)C6—N2—C5—N124.6 (5)
N5—Ni1—N1—C527.2 (12)C6—N2—C5—C4156.4 (4)
N1i—Ni1—N1—C549.8 (2)C3—C4—C5—N14.4 (6)
N3—Ni1—N1—C1155.6 (3)C3—C4—C5—N2176.6 (4)
N3i—Ni1—N1—C123.9 (3)C10—N3—C6—N2179.2 (3)
N5i—Ni1—N1—C163.4 (3)Ni1—N3—C6—N20.4 (4)
N5—Ni1—N1—C1171.5 (10)C10—N3—C6—C70.8 (5)
N1i—Ni1—N1—C1111.4 (3)Ni1—N3—C6—C7178.9 (3)
N3i—Ni1—N3—C6164.8 (2)C5—N2—C6—N339.5 (5)
N5i—Ni1—N3—C6118.3 (3)C5—N2—C6—C7142.0 (4)
N5—Ni1—N3—C6148.6 (3)N3—C6—C7—C80.3 (6)
N1i—Ni1—N3—C660.3 (3)N2—C6—C7—C8178.8 (3)
N1—Ni1—N3—C629.9 (3)C6—C7—C8—C90.6 (6)
N3i—Ni1—N3—C1015.5 (2)C7—C8—C9—C101.1 (6)
N5i—Ni1—N3—C1062.1 (3)C6—N3—C10—N4178.8 (3)
N5—Ni1—N3—C1031.0 (3)Ni1—N3—C10—N41.5 (4)
N1i—Ni1—N3—C10119.4 (2)C6—N3—C10—C90.2 (5)
N1—Ni1—N3—C10150.5 (3)Ni1—N3—C10—C9179.4 (3)
N3—Ni1—N5—C1143.1 (3)C11—N4—C10—N344.9 (5)
N3i—Ni1—N5—C11136.4 (3)C11—N4—C10—C9136.0 (4)
N5i—Ni1—N5—C1148.9 (2)C8—C9—C10—N30.7 (6)
N1i—Ni1—N5—C11136.2 (3)C8—C9—C10—N4179.7 (4)
N1—Ni1—N5—C1159.1 (12)C15—N5—C11—N4173.8 (3)
N3—Ni1—N5—C15152.7 (3)Ni1—N5—C11—N421.7 (4)
N3i—Ni1—N5—C1527.8 (3)C15—N5—C11—C125.2 (5)
N5i—Ni1—N5—C15115.3 (3)Ni1—N5—C11—C12159.3 (3)
N1i—Ni1—N5—C1559.6 (3)C10—N4—C11—N531.3 (5)
N1—Ni1—N5—C15136.7 (10)C10—N4—C11—C12147.6 (4)
C5—N1—C1—C26.0 (5)N5—C11—C12—C133.0 (7)
Ni1—N1—C1—C2155.7 (3)N4—C11—C12—C13176.0 (4)
N1—C1—C2—C30.3 (6)C11—C12—C13—C141.3 (7)
C1—C2—C3—C43.5 (6)C12—C13—C14—C153.0 (7)
C2—C3—C4—C51.6 (6)C13—C14—C15—N50.7 (6)
C1—N1—C5—N2173.0 (3)C11—N5—C15—C143.4 (5)
Ni1—N1—C5—N225.3 (4)Ni1—N5—C15—C14161.1 (3)
Symmetry code: (i) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2A···O10.862.122.911 (4)153
N4—H4A···O3ii0.862.343.170 (6)163
N4—H4A···O2ii0.862.403.109 (5)140
Symmetry code: (ii) x, y1, z.
 

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