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The title complex, [Ni(C5H5NO)(C9H18N4O3)(H2O)](NO3)2, is a six-coordinate pseudo-octahedral nickel(II) complex containing a tripodal amine ligand framework with three oxime donors, as well as pyridine N-oxide and aqua ligands. This complex displays crystallographic mirror symmetry and O—H...O hydrogen bonding between the cation and anion.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680403003X/lh6317sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680403003X/lh6317Isup2.hkl
Contains datablock I

CCDC reference: 258707

Key indicators

  • Single-crystal X-ray study
  • T = 294 K
  • Mean [sigma](C-C) = 0.005 Å
  • Disorder in solvent or counterion
  • R factor = 0.030
  • wR factor = 0.071
  • Data-to-parameter ratio = 14.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for N4 PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors for O5B PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for N5 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 20.00 Perc.
Alert level G REFLT03_ALERT_4_G WARNING: Large fraction of Friedel related reflns may be needed to determine absolute structure From the CIF: _diffrn_reflns_theta_max 29.40 From the CIF: _reflns_number_total 2547 Count of symmetry unique reflns 1736 Completeness (_total/calc) 146.72% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 811 Fraction of Friedel pairs measured 0.467 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 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 0 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Aqua(pyridine N-oxide-κO)[tris(2-hydroxyaminopropyl)amine-κ4N]nickel(II) dinitrate top
Crystal data top
[Ni(C5H5NO)(C9H18N4O3)(H2O)](NO3)2F(000) = 1096
Mr = 526.12Dx = 1.512 Mg m3
Orthorhombic, Cmc21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c -2Cell parameters from 5192 reflections
a = 11.0671 (10) Åθ = 2.7–29.4°
b = 14.0481 (10) ŵ = 0.91 mm1
c = 14.8625 (12) ÅT = 294 K
V = 2310.7 (3) Å3Block, purple
Z = 40.54 × 0.45 × 0.30 mm
Data collection top
Bruker SMART 1K CCD
diffractometer
2547 independent reflections
Radiation source: sealed tube2427 reflections with I > 2σ(I)'
Graphite monochromatorRint = 0.031
ω scansθmax = 29.4°, θmin = 2.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
h = 1415
Tmin = 0.634, Tmax = 0.765k = 1719
7484 measured reflectionsl = 2014
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.030H-atom parameters constrained
wR(F2) = 0.071 w = 1/[σ2(Fo2) + (0.0328P)2 + 1.1661P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.007
2547 reflectionsΔρmax = 0.27 e Å3
176 parametersΔρmin = 0.49 e Å3
1 restraintAbsolute structure: Flack (1983), 1736 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.065 (16)
Special details top

Experimental. The crystal was mounted on the tip of a glass fiber with epoxy resin.

The first 50 frames of data were recollected for a decay correction. The decay correction was applied simultaneously with the absorption correction in SADABS. No formal measure of the extent of decay is printed out by this program.

The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections above 20 σ(I).

Note that the absorption correction parameters Tmin and Tmax also reflect beam corrections, etc. As a result, the numerical values for Tmin and Tmax may differ from expected values based solely on absorption effects and crystal size.

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.

dihedral angle for the tilt of the pyridine-N-oxide ring is 90.0 (1)° for the planes defined as Ni/C4/O4 and N4/C7/C8/C9/C8A/C9A/O4

the least squares deviation for the pyridine-N-oxide ring defined as N4/C7/C8/C9/C8A/C9A/O4 is 0.0053 Å

symmetry operator to generate C8A and C9A = -x + 1, y, z

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*/UeqOcc. (<1)
Ni0.50000.35562 (2)0.75087 (2)0.02989 (9)
O10.50000.4926 (2)0.59124 (19)0.0634 (8)
H10.50000.42990.59250.095*
O20.22213 (16)0.33684 (14)0.71756 (13)0.0541 (5)
H20.23790.36110.65600.081*
O30.50000.22996 (19)0.82726 (19)0.0424 (6)
H30.44540.21940.86010.064*
O40.50000.28402 (17)0.63440 (18)0.0506 (7)
N10.50000.48143 (19)0.6845 (2)0.0377 (6)
N20.31744 (17)0.36694 (13)0.77257 (14)0.0378 (5)
N30.50000.4471 (2)0.8617 (2)0.0348 (6)
N40.50000.1892 (2)0.6360 (2)0.0474 (8)
C10.3876 (2)0.4239 (2)0.91275 (18)0.0448 (6)
H1A0.36310.47880.94780.054*
H1B0.40380.37200.95410.054*
C20.2870 (2)0.39592 (19)0.85031 (19)0.0430 (6)
C30.1600 (3)0.4009 (3)0.8834 (3)0.0750 (10)
H3A0.15100.36050.93500.112*
H3B0.10610.38020.83670.112*
H3C0.14110.46540.89970.112*
C40.50000.5468 (3)0.8296 (3)0.0498 (9)
H40.56960.57340.85210.060*
C50.50000.5583 (2)0.7298 (3)0.0402 (9)
C60.50000.6567 (3)0.6921 (4)0.0687 (14)
H6A0.45250.69750.73000.103*0.50
H6B0.46610.65570.63270.103*0.50
H6C0.58140.68010.68940.103*0.50
C70.3958 (4)0.1431 (2)0.6374 (3)0.0781 (12)
H70.32350.17690.63790.094*
C80.3946 (5)0.0450 (2)0.6380 (4)0.0971 (15)
H80.32130.01260.63800.117*
C90.50000.0045 (3)0.6388 (5)0.098 (2)
H90.50000.07300.64020.118*
N50.2180 (2)0.33290 (17)0.48815 (19)0.0564 (6)
O5A0.1840 (9)0.2617 (10)0.5250 (11)0.086 (3)0.50
O5B0.1328 (9)0.2859 (11)0.5225 (11)0.106 (4)0.50
O60.2124 (3)0.3444 (2)0.40607 (18)0.0850 (9)
O70.2827 (3)0.3821 (2)0.5357 (2)0.0854 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.03301 (16)0.02940 (15)0.02726 (17)0.0000.0000.00018 (19)
O10.107 (3)0.0487 (15)0.0348 (16)0.0000.0000.0085 (12)
O20.0430 (10)0.0636 (11)0.0557 (12)0.0054 (8)0.0180 (8)0.0048 (8)
O30.0450 (14)0.0481 (14)0.0341 (13)0.0000.0000.0098 (11)
O40.088 (2)0.0319 (12)0.0321 (14)0.0000.0000.0003 (10)
N10.0447 (15)0.0351 (14)0.0334 (16)0.0000.0000.0037 (12)
N20.0340 (8)0.0383 (9)0.0410 (14)0.0008 (7)0.0064 (8)0.0005 (7)
N30.0343 (13)0.0400 (14)0.0300 (15)0.0000.0000.0023 (12)
N40.076 (2)0.0337 (15)0.0329 (17)0.0000.0000.0015 (12)
C10.0387 (12)0.0584 (15)0.0374 (13)0.0007 (11)0.0042 (11)0.0065 (11)
C20.0292 (10)0.0527 (14)0.0470 (16)0.0005 (9)0.0015 (10)0.0017 (11)
C30.0358 (14)0.114 (3)0.075 (3)0.0015 (17)0.0126 (15)0.018 (2)
C40.060 (2)0.0391 (19)0.050 (2)0.0000.0000.0093 (17)
C50.0408 (15)0.0325 (14)0.047 (3)0.0000.0000.0040 (14)
C60.097 (4)0.0339 (19)0.075 (3)0.0000.0000.0082 (19)
C70.079 (2)0.0501 (17)0.105 (3)0.0053 (15)0.021 (2)0.0009 (18)
C80.109 (3)0.0470 (18)0.135 (4)0.0233 (19)0.029 (3)0.005 (2)
C90.166 (7)0.035 (2)0.093 (4)0.0000.0000.003 (2)
N50.0644 (16)0.0477 (12)0.0570 (17)0.0072 (11)0.0101 (13)0.0054 (11)
O5A0.095 (7)0.075 (5)0.089 (6)0.029 (5)0.018 (6)0.014 (4)
O5B0.106 (8)0.125 (11)0.088 (7)0.068 (7)0.020 (7)0.021 (7)
O60.100 (2)0.103 (2)0.0521 (16)0.0283 (16)0.0134 (15)0.0024 (13)
O70.0850 (18)0.1012 (19)0.0701 (18)0.0322 (15)0.0292 (15)0.0021 (14)
Geometric parameters (Å, º) top
Ni—O42.002 (3)C2—C31.491 (4)
Ni—N12.024 (3)C3—H3A0.9600
Ni—N22.0521 (19)C3—H3B0.9600
Ni—N32.089 (3)C3—H3C0.9600
Ni—O32.099 (3)C4—C51.492 (6)
O1—N11.395 (4)C4—H40.9185
O1—H10.8804C5—C61.491 (5)
O2—N21.400 (3)C6—H6A0.9600
O2—H20.9918C6—H6B0.9600
O3—H30.7908C6—H6C0.9600
O4—N41.333 (4)C7—C81.379 (4)
N1—C51.273 (5)C7—H70.9300
N2—C21.270 (3)C8—C91.358 (5)
N3—C41.480 (5)C8—H80.9300
N3—C11.493 (3)C9—H90.9626
N4—C71.322 (4)N5—O5A1.201 (14)
C1—C21.501 (4)N5—O71.220 (3)
C1—H1A0.9700N5—O61.232 (4)
C1—H1B0.9700N5—O5B1.259 (13)
O4—Ni—N190.98 (11)C2—C1—H1B109.4
O4—Ni—N2i100.07 (6)H1A—C1—H1B108.0
N1—Ni—N2i90.51 (5)N2—C2—C3124.4 (3)
O4—Ni—N2100.07 (6)N2—C2—C1116.7 (2)
N1—Ni—N290.51 (5)C3—C2—C1118.9 (3)
N2i—Ni—N2159.82 (11)C2—C3—H3A109.5
O4—Ni—N3172.19 (11)C2—C3—H3B109.5
N1—Ni—N381.20 (13)H3A—C3—H3B109.5
N2i—Ni—N380.12 (5)C2—C3—H3C109.5
N2—Ni—N380.12 (5)H3A—C3—H3C109.5
O4—Ni—O392.59 (11)H3B—C3—H3C109.5
N1—Ni—O3176.43 (13)N3—C4—C5115.0 (3)
N2i—Ni—O388.86 (6)N3—C4—H4105.5
N2—Ni—O388.87 (6)C5—C4—H4108.5
N3—Ni—O395.23 (11)N1—C5—C6125.9 (4)
N1—O1—H182.3N1—C5—C4115.8 (3)
N2—O2—H2107.6C6—C5—C4118.3 (3)
Ni—O3—H3119.4C5—C6—H6A109.5
N4—O4—Ni119.1 (2)C5—C6—H6B109.5
C5—N1—O1115.5 (3)H6A—C6—H6B109.5
C5—N1—Ni118.9 (3)C5—C6—H6C109.5
O1—N1—Ni125.6 (2)H6A—C6—H6C109.5
C2—N2—O2115.4 (2)H6B—C6—H6C109.5
C2—N2—Ni115.37 (16)N4—C7—C8119.9 (4)
O2—N2—Ni128.80 (15)N4—C7—H7120.1
C4—N3—C1i111.75 (18)C8—C7—H7120.1
C4—N3—C1111.75 (18)C9—C8—C7120.2 (4)
C1i—N3—C1112.8 (3)C9—C8—H8119.9
C4—N3—Ni109.2 (2)C7—C8—H8119.9
C1i—N3—Ni105.43 (16)C8i—C9—C8118.4 (4)
C1—N3—Ni105.44 (16)C8i—C9—H9120.8
C7—N4—C7i121.4 (4)C8—C9—H9120.8
C7—N4—O4119.31 (19)O5A—N5—O7113.0 (8)
C7i—N4—O4119.31 (19)O5A—N5—O6123.0 (8)
N3—C1—C2111.1 (2)O7—N5—O6122.0 (3)
N3—C1—H1A109.4O7—N5—O5B120.1 (8)
C2—C1—H1A109.4O6—N5—O5B115.6 (7)
N3—C1—H1B109.4
Symmetry code: (i) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···O40.882.142.999 (4)164
O2—H2···O70.991.882.856 (4)168
O2—H2···O5A0.992.473.080 (17)119
O2—H2···O5B0.992.533.146 (16)120
O3—H3···O6ii0.792.082.826 (3)158
O3—H3···O5Bii0.792.573.260 (15)148
Symmetry code: (ii) x+1/2, y+1/2, z+1/2.
 

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