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The title compound, [CuBr(C6H7NO)2]Br·H2O, is an ionic mononuclear complex in which the [CuBr(C6H7NO)2]+ cation possesses distorted square-pyramidal geometry. The CuII centre is coordinated by two neutral 2-(pyridin-2-yl)methanol (2-pyMeOH) ligands and a terminal bromide ligand. The 2-pyMeOH ligands are coordinated in a bidentate chelating manner through the pyridine N and hy­droxy O atoms, forming a five-membered chelate ring with the CuII centre. The planes of the pyridine rings are twisted by 58.71 (14)° with respect to each other. The charge is balanced by a noncoordinating bromide anion which, together with a solvent water mol­ecule, links the components through hydrogen bonds into infinite chains propagating along the a axis. The mononuclear cations appear to associate in pairs through weak interactions between the metal atom of one cation and the halogen atom of an adjacent cation.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113013437/sk3487sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270113013437/sk3487Isup2.hkl
Contains datablock I

CCDC reference: 950435

Comment top

The preparation of coordination polymers remains an attractive field of research in coordination chemistry. We have been interested for some time in the use of simple pyridyl-substituted alcohols as organic linker ligands (Lah et al., 2006; Lah & Leban, 2010; Lapanje et al., 2012; Trdin & Lah, 2012). During the course of the preparation of new CuII complexes with 2-(pyridin-2-yl)methanol (2-pyMeOH) and various carboxylic acids, the reaction of CuBr2 was carried out in methanol. Surprisingly, the resulting product did not contain any of the itaconic acid species that was present in the reaction mixture. Crystal structure determination revealed the product to be the title ionic compound, [CuBr(2-pyMeOH)2]Br.H2O, (I) (Fig. 1).

The [CuBr(C6H7NO)2]+ cation of (I) shows a distorted square-pyramidal geometry, in which the CuII centre is coordinated by two neutral and crystallographically distinct 2-pyMeOH molecules in a bidentate chelating manner, and a Br atom as a terminal ligand. The basal plane consists of the CuN2OBr chromophore; the axial site is occupied by the remaining O atom of one of the two 2-pyMeOH ligands. The charge is balanced by a noncoordinating bromide anion. Some geometric parameters are listed in Table 1.

In addition, the structure contains solvent water molecules which are involved in the formation of infinite hydrogen-bonded chains oriented along the a axis (Fig. 2). Each water molecule is a hydrogen-bond donor to two neighbouring bromide anions and a hydrogen-bond acceptor from the hydroxy group of one of the two distinct 2-pyMeOH ligands. The remaining hydroxy group is involved in hydrogen-bond formation with the bromide counterion. Thus, each noncoordinating bromide anion acts as an acceptor of three hydrogen bonds (Table 2). The chains are held together by weak ππ stacking interactions (Fig. 3).

In a comparison of the structure of (I) with those of known ionic halide complexes of transition metals with simple pyridine alcohols, six structures need to be mentioned. Three CuII complexes are reported as mononuclear ionic compounds with the stoichiometry [CuXL2]X: X = Cl and L = 2-pyMeOH (Antonioli et al., 2007), X = Cl and L = 2-pyEtOH (Hamamci et al., 2004), and X = Br and L = 2-pyEtOH (Lah & Leban, 2010). All three crystallize as anhydrous compounds and contain cations with a similar arrangement of ligands around the CuII centre. Three further structures deserve a closer look: (a) a chloride complex with 2-pyMeOH, described as a dinuclear ionic complex with a formulation of [Cu2Cl2(2-pyMeOH)4]Cl2.2H2O, (II) (Lah & Leban, 2010); (b) an analogous cobalt complex, [Co2Cl2(2-pyMeOH)4]Cl2.2H2O, (III) (Yilmaz et al., 2004); and (c) a chloride complex of CuII and the 4-bromo derivative of 2-pyMeOH with a formulation of [CuCl(2-pyMeOH)2]Cl.H2O, (IV) (Hubrich et al., 2010).

These last three compounds are closely related to (I) so that their unit-cell parameters agree reasonably well [allowing for the additional Br atom on the 2-pyMeOH ligand in (IV)]. A comparison of the unit-cell parameters is listed in Table 3. Nevertheless, two of them are described as dinuclear [(II) and (III)], while (IV) is described as a mononuclear ionic compound.

Closer inspection of the coordination environment in all the reported structures reveals that the M—X distances (M = metal cation and X = halogenide anion) vary from structure to structure (Table 4). A strong coordinative bond of the second halogen atom is only observed in the case of (III), whereas in the other structures a significant difference in M—X distances for the `bonded' halogenide anions is observed. Considering the sum of the van der Waals radii for the present atoms (Standard reference?), there is an attractive interaction between the metal centre and the halogenido atom of the neighbouring unit in (II) and (III), and the description of (IV) as a mononuclear ionic compound is justified. Being aware that, in (I), the M—Br distance (3.2128 (6) Å) is just below the sum of the van der Waals radii (3.25 Å), the structure described here can also be described as a dinuclear ionic compound with the formulation [Cu2Br2(2-pyMeOH)4]Br2.2H2O (Fig. 4).

Related literature top

For related literature, see: Antonioli et al. (2007); Hamamci et al. (2004); Hubrich et al. (2010); Lah & Leban (2010); Lah et al. (2006); Lapanje et al. (2012); Trdin & Lah (2012); Yilmaz et al. (2004).

Experimental top

CuBr2 (120 mg, 5.4 mmol) was dissolved in methanol (15 ml) while mixing and heating to boiling. Itaconic acid (2-methylidenebutanedioic acid; 70 mg, 5.4 mmol) and 2-pyMeOH (0,15 ml, 1.5 mmol) were added. The resulting solution was left under ambient conditions for slow evaporation of the solvent. Turquoise–blue crystals of (I) appeared within a few days.

Refinement top

All C-bound H atoms were initially found in a difference Fourier map, but they were repositioned at their calculated positions and refined using a riding model. Aromatic H atoms were permitted to ride, with C—H = 0.93 Å and Ueq(H) = 1.2Uiso(C), and those of the CH2 group were constrained, with C—H = 0.97 Å and Ueq(H)=1.2Uiso(C). The H atoms of the hydroxy groups and the water molecule were positioned from a difference Fourier map and refined freely.

Computing details top

Data collection: CrysAlis PRO (Agilent, 2011); cell refinement: CrysAlis PRO (Agilent, 2011); data reduction: CrysAlis PRO (Agilent, 2011); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, (2012); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. A view of (I), showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level.
[Figure 2] Fig. 2. Part of the crystal structure of (I), showing the formation of hydrogen-bonded chains. Hydrogen bonds are shown as dashed lines. (Colour key for the electronic version of the paper: water molecules are red, bromide counter-ions are orange spheres and complex cations are grey.)
[Figure 3] Fig. 3. A packing diagram for (I), showing the orientation of the hydrogen-bonded chains. Hydrogen bonds are shown as dashed lines.
[Figure 4] Fig. 4. A view of the assembly of two cations of (I) through weak Cu—Br interactions (dashed lines).
Bromidobis[2-(pyridin-2-yl)methanol-κ2N,O]copper(II) bromide monohydrate top
Crystal data top
[CuBr(C6H7NO)2]Br·H2OZ = 2
Mr = 459.63F(000) = 450
Triclinic, P1Dx = 1.915 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.9681 (6) ÅCell parameters from 3806 reflections
b = 9.8543 (6) Åθ = 2.9–30.4°
c = 11.1812 (8) ŵ = 6.39 mm1
α = 74.974 (6)°T = 150 K
β = 72.481 (6)°Prismatic, light blue
γ = 76.590 (6)°0.3 × 0.2 × 0.2 mm
V = 797.24 (10) Å3
Data collection top
Agilent SuperNova (Dual, Cu at zero, Atlas)
diffractometer
3668 independent reflections
Radiation source: SuperNova (Mo) X-ray Source3086 reflections with I > 2σ(I)
Mirror monochromatorRint = 0.037
Detector resolution: 10.4933 pixels mm-1θmax = 27.5°, θmin = 2.9°
ω scansh = 109
Absorption correction: multi-scan
(CrysAlis PRO; Agilent, 2011)
k = 1212
Tmin = 0.073, Tmax = 1.000l = 1414
6592 measured reflections
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)] = 0.041Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.092H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.0382P)2]
where P = (Fo2 + 2Fc2)/3
3668 reflections(Δ/σ)max = 0.001
197 parametersΔρmax = 0.92 e Å3
0 restraintsΔρmin = 0.85 e Å3
Crystal data top
[CuBr(C6H7NO)2]Br·H2Oγ = 76.590 (6)°
Mr = 459.63V = 797.24 (10) Å3
Triclinic, P1Z = 2
a = 7.9681 (6) ÅMo Kα radiation
b = 9.8543 (6) ŵ = 6.39 mm1
c = 11.1812 (8) ÅT = 150 K
α = 74.974 (6)°0.3 × 0.2 × 0.2 mm
β = 72.481 (6)°
Data collection top
Agilent SuperNova (Dual, Cu at zero, Atlas)
diffractometer
3668 independent reflections
Absorption correction: multi-scan
(CrysAlis PRO; Agilent, 2011)
3086 reflections with I > 2σ(I)
Tmin = 0.073, Tmax = 1.000Rint = 0.037
6592 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0410 restraints
wR(F2) = 0.092H atoms treated by a mixture of independent and constrained refinement
S = 1.04Δρmax = 0.92 e Å3
3668 reflectionsΔρmin = 0.85 e Å3
197 parameters
Special details top

Experimental. Abdorption correction: CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.

Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'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
Br10.69276 (5)0.11173 (4)0.41782 (4)0.02072 (12)
Br20.82213 (5)0.33174 (4)0.01707 (4)0.02657 (13)
Cu10.41848 (6)0.15156 (4)0.35337 (4)0.01644 (13)
O2B0.1749 (4)0.1436 (3)0.3342 (3)0.0216 (6)
O2A0.4565 (4)0.3461 (3)0.1964 (3)0.0233 (6)
O1W1.0781 (5)0.3461 (4)0.1580 (3)0.0412 (9)
H1W1.120 (7)0.408 (5)0.117 (4)0.033 (15)*
H2W1.000 (9)0.344 (6)0.122 (5)0.065 (19)*
N210.4958 (4)0.0118 (3)0.2393 (3)0.0165 (6)
C220.3623 (5)0.0388 (4)0.2233 (3)0.0186 (8)
C250.7064 (6)0.1302 (4)0.0995 (4)0.0284 (9)
H250.82430.15910.05730.034*
N110.3099 (4)0.3101 (3)0.4460 (3)0.0174 (6)
C240.5702 (6)0.1840 (4)0.0866 (4)0.0292 (10)
H240.59520.25190.03670.035*
C1B0.1767 (5)0.0183 (4)0.2924 (4)0.0243 (9)
H1B10.09850.04020.23570.029*
H1B20.13220.05360.36580.029*
C260.6636 (6)0.0318 (4)0.1770 (4)0.0241 (9)
H260.75510.00540.18620.029*
C120.3498 (5)0.4406 (4)0.3872 (4)0.0212 (8)
C140.1854 (6)0.5329 (4)0.5740 (4)0.0282 (9)
H140.14500.60810.61700.034*
C150.1414 (6)0.3995 (4)0.6338 (4)0.0278 (9)
H150.06980.38340.71710.033*
C130.2896 (6)0.5526 (4)0.4504 (4)0.0273 (9)
H130.31980.64180.40900.033*
C1A0.4647 (6)0.4577 (4)0.2527 (4)0.0262 (9)
H1A10.42390.54920.20290.031*
H1A20.58710.45520.25270.031*
C160.2069 (5)0.2909 (4)0.5663 (4)0.0234 (8)
H160.17830.20090.60600.028*
C230.3979 (6)0.1375 (4)0.1472 (4)0.0260 (9)
H230.30490.17220.13730.031*
H2A0.542 (7)0.346 (5)0.139 (4)0.032 (14)*
H2B0.149 (6)0.203 (4)0.288 (4)0.017 (13)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br10.0136 (2)0.0230 (2)0.0271 (2)0.00025 (15)0.00721 (18)0.00840 (16)
Br20.0208 (2)0.0361 (2)0.0236 (2)0.00661 (18)0.00253 (19)0.00954 (18)
Cu10.0117 (2)0.0178 (2)0.0205 (3)0.00292 (18)0.0042 (2)0.00993 (18)
O2B0.0158 (14)0.0239 (15)0.0269 (16)0.0029 (12)0.0088 (14)0.0101 (13)
O2A0.0216 (16)0.0280 (15)0.0184 (15)0.0041 (12)0.0019 (15)0.0097 (12)
O1W0.053 (2)0.0335 (19)0.047 (2)0.0148 (18)0.032 (2)0.0030 (17)
N210.0157 (16)0.0164 (15)0.0160 (15)0.0014 (12)0.0043 (14)0.0043 (12)
C220.024 (2)0.0152 (18)0.0172 (18)0.0002 (15)0.0082 (18)0.0032 (14)
C250.029 (2)0.030 (2)0.017 (2)0.0125 (18)0.002 (2)0.0089 (17)
N110.0127 (16)0.0185 (16)0.0198 (16)0.0021 (12)0.0024 (15)0.0082 (13)
C240.048 (3)0.018 (2)0.022 (2)0.0029 (19)0.011 (2)0.0094 (16)
C1B0.017 (2)0.027 (2)0.031 (2)0.0027 (16)0.007 (2)0.0103 (18)
C260.021 (2)0.026 (2)0.021 (2)0.0029 (17)0.0044 (19)0.0058 (16)
C120.017 (2)0.0212 (19)0.023 (2)0.0016 (16)0.0070 (18)0.0039 (16)
C140.028 (2)0.027 (2)0.031 (2)0.0087 (18)0.009 (2)0.0185 (18)
C150.027 (2)0.032 (2)0.020 (2)0.0051 (18)0.001 (2)0.0138 (17)
C130.029 (2)0.0173 (19)0.037 (2)0.0002 (17)0.009 (2)0.0094 (17)
C1A0.028 (2)0.022 (2)0.026 (2)0.0070 (17)0.000 (2)0.0061 (17)
C160.021 (2)0.022 (2)0.024 (2)0.0009 (16)0.0022 (19)0.0063 (16)
C230.039 (3)0.0183 (19)0.025 (2)0.0054 (18)0.011 (2)0.0066 (16)
Geometric parameters (Å, º) top
Br1—Cu12.4194 (6)N11—C161.339 (5)
Cu1—N111.983 (3)N11—C121.346 (4)
Cu1—N211.987 (3)C24—C231.365 (6)
Cu1—O2B2.037 (3)C24—H240.9300
Cu1—O2A2.247 (3)C1B—H1B10.9700
Cu1—Br1i3.2129 (6)C1B—H1B20.9700
O2B—C1B1.425 (4)C26—H260.9300
O2B—H2B0.71 (4)C12—C131.379 (5)
O2A—C1A1.424 (4)C12—C1A1.497 (5)
O2A—H2A0.78 (5)C14—C131.372 (6)
O1W—H1W0.75 (5)C14—C151.383 (6)
O1W—H2W0.84 (6)C14—H140.9300
N21—C261.336 (5)C15—C161.382 (5)
N21—C221.348 (4)C15—H150.9300
C22—C231.381 (5)C13—H130.9300
C22—C1B1.501 (5)C1A—H1A10.9700
C25—C241.371 (6)C1A—H1A20.9700
C25—C261.382 (5)C16—H160.9300
C25—H250.9300C23—H230.9300
N11—Cu1—N21168.98 (12)C23—C24—H24120.1
N11—Cu1—O2B90.14 (11)C25—C24—H24120.1
N21—Cu1—O2B81.45 (12)O2B—C1B—C22110.7 (3)
N11—Cu1—O2A77.10 (11)O2B—C1B—H1B1109.5
N21—Cu1—O2A96.24 (11)C22—C1B—H1B1109.5
O2B—Cu1—O2A93.69 (11)O2B—C1B—H1B2109.5
N11—Cu1—Br192.47 (8)C22—C1B—H1B2109.5
N21—Cu1—Br197.41 (9)H1B1—C1B—H1B2108.1
O2B—Cu1—Br1166.09 (9)N21—C26—C25122.5 (4)
O2A—Cu1—Br1100.21 (7)N21—C26—H26118.7
N11—Cu1—Br1i99.40 (9)C25—C26—H26118.7
N21—Cu1—Br1i86.10 (8)N11—C12—C13120.8 (3)
O2B—Cu1—Br1i79.31 (9)N11—C12—C1A117.4 (3)
O2A—Cu1—Br1i172.24 (8)C13—C12—C1A121.8 (3)
Br1—Cu1—Br1i86.785 (17)C13—C14—C15119.1 (4)
C1B—O2B—Cu1111.7 (2)C13—C14—H14120.5
C1B—O2B—H2B107 (3)C15—C14—H14120.5
Cu1—O2B—H2B110 (3)C16—C15—C14118.2 (4)
C1A—O2A—Cu1107.5 (2)C16—C15—H15120.9
C1A—O2A—H2A104 (3)C14—C15—H15120.9
Cu1—O2A—H2A121 (3)C14—C13—C12120.2 (4)
H1W—O1W—H2W103 (5)C14—C13—H13119.9
C26—N21—C22118.9 (3)C12—C13—H13119.9
C26—N21—Cu1126.1 (2)O2A—C1A—C12109.8 (3)
C22—N21—Cu1115.0 (2)O2A—C1A—H1A1109.7
N21—C22—C23120.8 (4)C12—C1A—H1A1109.7
N21—C22—C1B116.2 (3)O2A—C1A—H1A2109.7
C23—C22—C1B123.0 (3)C12—C1A—H1A2109.7
C24—C25—C26118.2 (4)H1A1—C1A—H1A2108.2
C24—C25—H25120.9N11—C16—C15122.7 (4)
C26—C25—H25120.9N11—C16—H16118.7
C16—N11—C12119.0 (3)C15—C16—H16118.7
C16—N11—Cu1122.7 (2)C24—C23—C22119.7 (4)
C12—N11—Cu1118.2 (2)C24—C23—H23120.2
C23—C24—C25119.8 (4)C22—C23—H23120.2
Symmetry code: (i) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2B—H2B···O1Wii0.71 (4)1.86 (4)2.573 (5)175 (5)
O2A—H2A···Br20.78 (5)2.39 (5)3.163 (3)173 (4)
O1W—H1W···Br2iii0.75 (5)2.60 (5)3.319 (4)162 (5)
O1W—H2W···Br20.84 (6)2.44 (6)3.271 (3)169 (5)
Symmetry codes: (ii) x1, y, z; (iii) x+2, y+1, z.

Experimental details

Crystal data
Chemical formula[CuBr(C6H7NO)2]Br·H2O
Mr459.63
Crystal system, space groupTriclinic, P1
Temperature (K)150
a, b, c (Å)7.9681 (6), 9.8543 (6), 11.1812 (8)
α, β, γ (°)74.974 (6), 72.481 (6), 76.590 (6)
V3)797.24 (10)
Z2
Radiation typeMo Kα
µ (mm1)6.39
Crystal size (mm)0.3 × 0.2 × 0.2
Data collection
DiffractometerAgilent SuperNova (Dual, Cu at zero, Atlas)
diffractometer
Absorption correctionMulti-scan
(CrysAlis PRO; Agilent, 2011)
Tmin, Tmax0.073, 1.000
No. of measured, independent and
observed [I > 2σ(I)] reflections
6592, 3668, 3086
Rint0.037
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.041, 0.092, 1.04
No. of reflections3668
No. of parameters197
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.92, 0.85

Computer programs: CrysAlis PRO (Agilent, 2011), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, (2012).

Selected geometric parameters (Å, º) top
Br1—Cu12.4194 (6)Cu1—O2B2.037 (3)
Cu1—N111.983 (3)Cu1—O2A2.247 (3)
Cu1—N211.987 (3)Cu1—Br1i3.2129 (6)
N11—Cu1—N21168.98 (12)O2B—Cu1—Br1166.09 (9)
N11—Cu1—O2B90.14 (11)O2A—Cu1—Br1100.21 (7)
N21—Cu1—O2B81.45 (12)N11—Cu1—Br1i99.40 (9)
N11—Cu1—O2A77.10 (11)N21—Cu1—Br1i86.10 (8)
N21—Cu1—O2A96.24 (11)O2B—Cu1—Br1i79.31 (9)
O2B—Cu1—O2A93.69 (11)O2A—Cu1—Br1i172.24 (8)
N11—Cu1—Br192.47 (8)Br1—Cu1—Br1i86.785 (17)
N21—Cu1—Br197.41 (9)
Symmetry code: (i) x+1, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O2B—H2B···O1Wii0.71 (4)1.86 (4)2.573 (5)175 (5)
O2A—H2A···Br20.78 (5)2.39 (5)3.163 (3)173 (4)
O1W—H1W···Br2iii0.75 (5)2.60 (5)3.319 (4)162 (5)
O1W—H2W···Br20.84 (6)2.44 (6)3.271 (3)169 (5)
Symmetry codes: (ii) x1, y, z; (iii) x+2, y+1, z.
Comparison of unit-cell parameters of (I) with those of the related compounds (II), (III) and (IV) top
(I)(II)(III)(IV)
T (K)15015013390
a (Å)7.9681 (6)7.71430 (10)7.9154 (6)7.9333 (3)
b (Å)9.8543 (6)9.7359 (2)9.5718 (6)11.1019 (3)
c (°)11.1812 (8)11.0072 (2)11.1614 (8)11.2436 (4)
α (°)74.974 (6)74.570 (1)72.121 (3)102.670 (2)
β (°)72.481 (6)72.311 (1)70.460 (3)102.670 (2)
γ (°)76.590 (6)77.405 (1)76.231 (3)101.724 (1)
V3)797.24 (10)750.71 (2)749.77 (9)862.52 (5)
Comparison of the coordination environment of the metal centre in (I) with those reported for the related compounds (II), (III) and (IV) top
(I)(II)(III)(IV)
M—N (Å)1.984 (3)1.9883 (13)2.0988 (8)1.97282)
1.987 (3)1.9858 (13)2.1004 (8)1.971 (2)
M—O (Å)2.0384 (3)2.0382 (12)2.1209 (7)2.029 (2)
2.2487 (3)2.2466 (4)2.1224 (8)2.179 (2)
MX (Å)2.4194 (2)2.2764 (4)2.4212 (3)2.2581 (2)
3.2129 (6)3.0434 (5)2.4620 (3)3.475 (5)
 

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