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In the title complex, [Ni(C10H10N4)3](NO3)2, the cation has crystallographic R32 symmetry while the anion lies on a threefold axis. In the cation, the NiII atom is coordinated by six N atoms from three 6,6′-diamino-2,2′-bipyridine ligands. In the crystal structure, a two-dimensional network is formed via inter­molecular N—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806026304/lh2115sup1.cif
Contains datablocks I, 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806026304/lh2115Isup2.hkl
Contains datablock I

CCDC reference: 618267

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.061
  • wR factor = 0.099
  • Data-to-parameter ratio = 13.5

checkCIF/PLATON results

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Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.13 Ratio
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.99 From the CIF: _reflns_number_total 1056 Count of symmetry unique reflns 592 Completeness (_total/calc) 178.38% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 464 Fraction of Friedel pairs measured 0.784 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 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 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

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

(I) top
Crystal data top
[Ni(C10H10N4)3](NO3)2Dx = 1.537 Mg m3
Mr = 741.39Mo Kα radiation, λ = 0.71073 Å
Trigonal, R32Cell parameters from 523 reflections
Hall symbol: R 3 2"θ = 2.2–17.6°
a = 14.537 (2) ŵ = 0.68 mm1
c = 13.125 (4) ÅT = 293 K
V = 2402.2 (9) Å3Prism, yellow
Z = 30.13 × 0.13 × 0.05 mm
F(000) = 1152
Data collection top
Bruker Smart APEX CCD
diffractometer
1056 independent reflections
Radiation source: fine-focus sealed tube890 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.088
φ and ω scansθmax = 26.0°, θmin = 2.2°
Absorption correction: multi-scan
SADABS (Sheldrick, 1996)
h = 1717
Tmin = 0.917, Tmax = 0.967k = 1117
4515 measured reflectionsl = 1516
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.061H-atom parameters constrained
wR(F2) = 0.099 w = 1/[σ2(Fo2) + (0.0322P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max < 0.001
1056 reflectionsΔρmax = 0.64 e Å3
78 parametersΔρmin = 0.35 e Å3
0 restraintsAbsolute structure: Flack (1983), 462 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.09 (4)
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
Ni10.33330.66670.16670.0290 (4)
N10.2716 (4)0.5250 (2)0.0856 (2)0.0379 (9)
C30.1480 (6)0.3151 (4)0.0321 (4)0.0642 (15)
H30.10660.24430.01310.077*
C40.2200 (4)0.3416 (4)0.1111 (4)0.0486 (13)
C10.1978 (4)0.4963 (5)0.0134 (4)0.0521 (14)
H10.18660.54800.01650.063*
C50.2896 (3)0.4510 (3)0.1295 (3)0.0388 (12)
N20.2210 (4)0.2636 (3)0.1679 (4)0.0775 (16)
H2A0.17690.19790.15460.093*
H2B0.26570.28000.21710.093*
C20.1366 (4)0.3910 (5)0.0187 (4)0.0632 (16)
H20.08950.37300.07300.076*
N30.00000.00000.1220 (4)0.0465 (14)
O10.0969 (3)0.0310 (3)0.1224 (3)0.0698 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0267 (5)0.0267 (5)0.0335 (7)0.0134 (2)0.0000.000
N10.038 (3)0.0382 (19)0.043 (2)0.023 (2)0.004 (2)0.0047 (14)
C30.052 (4)0.041 (3)0.088 (4)0.014 (4)0.011 (4)0.022 (3)
C40.039 (3)0.037 (3)0.066 (3)0.015 (2)0.002 (3)0.007 (3)
C10.047 (3)0.056 (3)0.055 (4)0.028 (3)0.011 (3)0.005 (3)
C50.034 (3)0.031 (3)0.050 (3)0.016 (2)0.002 (2)0.006 (2)
N20.061 (3)0.029 (2)0.129 (4)0.013 (2)0.016 (3)0.006 (3)
C20.050 (4)0.062 (4)0.062 (4)0.017 (3)0.026 (3)0.021 (3)
N30.047 (2)0.047 (2)0.046 (3)0.0234 (11)0.0000.000
O10.0430 (19)0.065 (3)0.102 (3)0.027 (2)0.0014 (18)0.004 (2)
Geometric parameters (Å, º) top
Ni1—N1i2.081 (3)C4—N21.364 (6)
Ni1—N1ii2.081 (3)C4—C51.415 (6)
Ni1—N12.081 (3)C1—C21.397 (7)
Ni1—N1iii2.081 (3)C1—H10.9300
Ni1—N1iv2.081 (3)C5—C5i1.471 (8)
Ni1—N1v2.081 (3)N2—H2A0.8600
N1—C11.333 (6)N2—H2B0.8600
N1—C51.356 (5)C2—H20.9300
C3—C21.369 (8)N3—O1vi1.245 (3)
C3—C41.383 (7)N3—O11.245 (3)
C3—H30.9300N3—O1vii1.245 (3)
N1i—Ni1—N1ii172.7 (3)C4—C3—H3119.3
N1i—Ni1—N178.6 (3)N2—C4—C3119.9 (5)
N1ii—Ni1—N196.18 (12)N2—C4—C5122.8 (5)
N1i—Ni1—N1iii89.5 (2)C3—C4—C5117.2 (4)
N1ii—Ni1—N1iii96.18 (12)N1—C1—C2121.9 (5)
N1—Ni1—N1iii96.18 (12)N1—C1—H1119.0
N1i—Ni1—N1iv96.18 (12)C2—C1—H1119.0
N1ii—Ni1—N1iv89.5 (2)N1—C5—C4120.4 (4)
N1—Ni1—N1iv172.7 (3)N1—C5—C5i114.0 (3)
N1iii—Ni1—N1iv78.6 (3)C4—C5—C5i125.3 (3)
N1i—Ni1—N1v96.18 (12)C4—N2—H2A120.0
N1ii—Ni1—N1v78.6 (3)C4—N2—H2B120.0
N1—Ni1—N1v89.5 (2)H2A—N2—H2B120.0
N1iii—Ni1—N1v172.7 (3)C3—C2—C1118.0 (5)
N1iv—Ni1—N1v96.18 (12)C3—C2—H2121.0
C1—N1—C5119.9 (4)C1—C2—H2121.0
C1—N1—Ni1123.7 (4)O1vi—N3—O1119.998 (6)
C5—N1—Ni1114.1 (3)O1vi—N3—O1vii119.998 (6)
C2—C3—C4121.4 (4)O1—N3—O1vii119.998 (6)
C2—C3—H3119.3
N1i—Ni1—N1—C1170.0 (5)Ni1—N1—C1—C2161.3 (4)
N1ii—Ni1—N1—C14.8 (4)C1—N1—C5—C49.8 (7)
N1iii—Ni1—N1—C1101.8 (3)Ni1—N1—C5—C4153.6 (3)
N1v—Ni1—N1—C173.6 (4)C1—N1—C5—C5i176.8 (5)
N1i—Ni1—N1—C57.3 (2)Ni1—N1—C5—C5i19.8 (6)
N1ii—Ni1—N1—C5167.5 (4)N2—C4—C5—N1166.4 (5)
N1iii—Ni1—N1—C595.5 (4)C3—C4—C5—N113.0 (7)
N1v—Ni1—N1—C589.1 (3)N2—C4—C5—C5i6.1 (8)
C2—C3—C4—N2172.4 (6)C3—C4—C5—C5i174.5 (6)
C2—C3—C4—C57.1 (8)C4—C3—C2—C11.8 (9)
C5—N1—C1—C20.5 (7)N1—C1—C2—C35.4 (8)
Symmetry codes: (i) x+2/3, x+y+1/3, z+1/3; (ii) x+y, x+1, z; (iii) y+1, xy+1, z; (iv) xy+2/3, y+4/3, z+1/3; (v) y1/3, x+1/3, z+1/3; (vi) x+y, x, z; (vii) y, xy, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2B···N2i0.862.372.829 (9)114
Symmetry code: (i) x+2/3, x+y+1/3, z+1/3.
 

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