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Acta Cryst. (2008). E64, m68    [ doi:10.1107/S1600536807059211 ]

Azido(methanol)[N,N'-(o-phenylene)bis(pyridine-2-carboxamidato)]manganese(III)

Y. Feng and D. Liao

Abstract top

In the title complex, [Mn(C18H12N4O2)(N3)(CH4O)], the MnIII ion is in a distorted octahedral coordination environment. In the crystal structure, intermolecular O-H...O hydrogen bonds connect molecules into centrosymmetric dimers.

Comment top

The planar tetradentate ligand bpb2-, bpb = 1,2-bis(pyridine-2-carboxamido)benzene, can coordinate four equatorial sites of six-coordinated paramagnetic cations, leaving two free axial positions to be occupied by bridging ligands. It is hence, one of the ideal candidates to act as a co-ligand for constructing expanded structures (Colacio et al., 2005; Ni, Kou, Zheng et al., 2005; Ni, Kou, Zhang et al., 2005; Ni, Kou, Zhao et al., 2005; Dominguez-Vera et al., 2005; Havranek et al., 1999; Lin et al., 2003; Liang et al., 2007; Zhang et al., 2006). Mn(III) compounds, with a high-spin ground state related to the Mn(III) ion (S = 2) and an apparent magnetic anisotropy of hexacoordinated Mn(III) centres due to Jahn—Teller distortion, usually display appealing magnetic properties (Lecren et al., 2007).

We originally attempted to synthesize complexes featuring azido-bridged Mn(III) metal chains by reaction of the [Mn(III)(bpb)]2- building blocks with NaN3. But, we fortuitously obtained title compound (I), and we report herein its crystal structure.

Related literature top

For general background, see: Ni, Kou, Zheng et al. (2005); Ni, Kou, Zhang et al. (2005); Ni, Kou, Zhao et al. (2005); Colacio et al. (2005); Dominguez-Vera et al. (2005); For bond-length data, see: Havranek et al. (1999); Lin et al. (2003); Liang et al. (2007). For related literature, see: Lecren et al. (2007); Zhang et al. (2006).

Experimental top

To a solution of [Mn(bpb)Cl(H2O)] (0.425 g, 1 mmol) in 20 ml of methanol was added a solution of NaN3 (0.065 g, 1 mmol) in a minimum volume of H2O. After stirring for 30 min at room temperature, the dark brown solution was filtered and allowed to stand for about one month at room temperature to form dark brown crystals of 1, [Mn(bpb)(N3)(CH3OH)]. The crystals were collected by suction filtration, washed with a minimum amount of water, and dried in vacuo. Elemental analysis: C19H16MnN7O2, Calcd: C 51.25%, H 3.62%, N 22.02%, Found: C 51.68%, H 3.87%, N 22.35%.. IR (KBr): 2035 cm-1 (N3-), 1622 cm-1 (C=O).

Refinement top

The H atom bonded to the O atom was located in a difference map and refined isotropically with a distance restraints of O—H = 0.84 (2) Å. Other H atoms were positioned geometrically and refined using a riding model (including free rotation about the ethanol C—C bond), with C—H = 0.93–0.96 Å and with Uiso(H) = 1.2 (1.5 for methyl group) times Ueq(C).

Computing details top

Data collection: CrystalClear (Rigaku, 2001); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker (1997); software used to prepare material for publication: CrystalStructure (Rigaku, 2001).

Figures top
[Figure 1] Fig. 1. The molecular structure with atom labels and 30% probability displacement ellipsoids for non-H atoms.
[Figure 2] Fig. 2. A centrostmmetric hydrogen-bonded dimer with the donor-acceptor distances shown as dashed lines [symmetry code: (A) -x, -y + 1, -z].
Azido(methanol)[N,N'-(o-phenylene)bis(pyridine-2-carboxamidato)]manganese(III) top
Crystal data top
[Mn(C18H12N4O2)(N3)(CH4O)]F000 = 912
Mr = 445.33Dx = 1.543 Mg m−3
Monoclinic, P21/cMo Kα radiation
λ = 0.71070 Å
Hall symbol: -P 2ybcCell parameters from 3879 reflections
a = 12.115 (2) Åθ = 1.2–27.8º
b = 9.4987 (19) ŵ = 0.73 mm−1
c = 16.748 (3) ÅT = 293 (2) K
β = 95.94 (3)ºPrim, red
V = 1917.0 (6) Å30.14 × 0.14 × 0.14 mm
Z = 4
Data collection top
Rigaku Saturn
diffractometer		3406 independent reflections
Radiation source: fine-focus sealed tube2957 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.061
Detector resolution: 7.31 pixels mm-1θmax = 25.1º
T = 293(2) Kθmin = 2.5º
ω scansh = −14→14
Absorption correction: multi-scan
(Jacobson, 1998)		k = −11→11
Tmin = 0.905, Tmax = 0.905l = −19→19
15658 measured reflections
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)] = 0.060H atoms treated by a mixture of
independent and constrained refinement
wR(F2) = 0.159  w = 1/[σ2(Fo2) + (0.0859P)2 + 0.7977P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max < 0.001
3406 reflectionsΔρmax = 0.47 e Å−3
269 parametersΔρmin = −0.52 e Å−3
7 restraintsExtinction correction: none
Primary atom site location: structure-invariant direct methods
Crystal data top
[Mn(C18H12N4O2)(N3)(CH4O)]V = 1917.0 (6) Å3
Mr = 445.33Z = 4
Monoclinic, P21/cMo Kα
a = 12.115 (2) ŵ = 0.73 mm−1
b = 9.4987 (19) ÅT = 293 (2) K
c = 16.748 (3) Å0.14 × 0.14 × 0.14 mm
β = 95.94 (3)º
Data collection top
Rigaku Saturn
diffractometer		3406 independent reflections
Absorption correction: multi-scan
(Jacobson, 1998)		2957 reflections with I > 2σ(I)
Tmin = 0.905, Tmax = 0.905Rint = 0.061
15658 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0607 restraints
wR(F2) = 0.159H atoms treated by a mixture of
independent and constrained refinement
S = 1.07Δρmax = 0.47 e Å−3
3406 reflectionsΔρmin = −0.52 e Å−3
269 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mn10.28436 (4)0.43236 (5)0.07581 (3)0.0426 (2)
N10.4102 (2)0.2866 (3)0.09158 (17)0.0457 (7)
N20.2637 (2)0.3704 (3)0.18327 (17)0.0475 (7)
N30.1504 (2)0.5370 (3)0.08979 (18)0.0457 (7)
N40.2560 (2)0.5208 (3)−0.03746 (17)0.0446 (7)
N50.4047 (3)0.5963 (4)0.10720 (19)0.0547 (6)
N60.3766 (3)0.7072 (4)0.12232 (18)0.0547 (6)
N70.3505 (5)0.8221 (5)0.1379 (3)0.1030 (15)
O10.3481 (3)0.2476 (3)0.29189 (17)0.0692 (8)
O20.0275 (2)0.7020 (3)0.03047 (18)0.0723 (9)
O30.1885 (3)0.2409 (3)0.01209 (19)0.0651 (8)
H0.1217 (19)0.269 (7)0.008 (4)0.14 (3)*
C190.1894 (5)0.0937 (5)0.0353 (4)0.0912 (17)
H19A0.14150.0413−0.00310.137*
H19B0.16370.08480.08740.137*
H19C0.26360.05750.03690.137*
C170.2895 (4)0.5841 (4)−0.1701 (2)0.0584 (10)
H17A0.33090.5721−0.21340.070*
C140.1715 (3)0.6137 (4)−0.0417 (2)0.0479 (9)
C90.0439 (4)0.4628 (4)0.3157 (3)0.0624 (11)
H9A0.02120.44310.36590.075*
C20.5578 (3)0.1396 (4)0.0584 (3)0.0574 (10)
H2A0.60320.10860.02040.069*
C40.5005 (3)0.1313 (4)0.1897 (2)0.0536 (10)
H4A0.50730.09530.24160.064*
C80.1394 (4)0.4006 (4)0.2927 (3)0.0579 (10)
H8A0.18150.34060.32760.069*
C60.3408 (3)0.2842 (4)0.2216 (2)0.0479 (9)
C10−0.0179 (4)0.5543 (4)0.2643 (3)0.0638 (12)
H10A−0.08150.59570.28030.077*
C160.2034 (4)0.6788 (5)−0.1744 (3)0.0659 (12)
H16A0.18590.7320−0.22060.079*
C150.1430 (4)0.6940 (4)−0.1093 (3)0.0629 (11)
H15A0.08420.7572−0.11100.075*
C30.5692 (3)0.0850 (4)0.1344 (3)0.0592 (11)
H3A0.62300.01710.14870.071*
C180.3139 (3)0.5069 (4)−0.1007 (2)0.0519 (9)
H18A0.37250.4433−0.09780.062*
C120.1084 (3)0.5218 (4)0.1652 (2)0.0470 (8)
C10.4782 (3)0.2411 (4)0.0387 (2)0.0543 (10)
H1A0.47140.2791−0.01270.065*
C110.0140 (3)0.5842 (4)0.1899 (3)0.0577 (10)
H11A−0.02750.64640.15600.069*
C130.1080 (3)0.6216 (4)0.0299 (2)0.0518 (9)
C70.1716 (3)0.4288 (4)0.2169 (2)0.0463 (9)
C50.4215 (3)0.2321 (4)0.1666 (2)0.0438 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0434 (4)0.0411 (4)0.0427 (4)0.0090 (2)0.0012 (2)0.0035 (2)
N10.0429 (16)0.0452 (17)0.0479 (17)0.0029 (13)−0.0007 (13)0.0035 (14)
N20.0507 (18)0.0436 (17)0.0488 (17)0.0073 (14)0.0079 (14)0.0056 (14)
N30.0446 (16)0.0414 (16)0.0502 (17)0.0054 (13)0.0002 (13)0.0015 (13)
N40.0480 (17)0.0396 (16)0.0438 (16)0.0042 (13)−0.0074 (13)0.0001 (13)
N50.0579 (14)0.0584 (15)0.0468 (13)−0.0053 (13)0.0012 (10)0.0014 (13)
N60.0579 (14)0.0584 (15)0.0468 (13)−0.0053 (13)0.0012 (10)0.0014 (13)
N70.125 (3)0.075 (3)0.111 (3)0.007 (3)0.020 (3)−0.013 (2)
O10.079 (2)0.076 (2)0.0525 (17)0.0197 (16)0.0103 (14)0.0191 (15)
O20.0586 (18)0.075 (2)0.081 (2)0.0288 (16)−0.0044 (15)0.0049 (16)
O30.0572 (18)0.0463 (16)0.088 (2)0.0060 (14)−0.0097 (15)0.0000 (14)
C190.073 (3)0.066 (3)0.128 (5)0.010 (3)−0.019 (3)0.010 (3)
C170.072 (3)0.055 (2)0.047 (2)−0.004 (2)−0.0016 (19)0.0044 (18)
C140.050 (2)0.0401 (19)0.051 (2)0.0023 (16)−0.0084 (16)0.0009 (16)
C90.064 (3)0.056 (2)0.071 (3)−0.010 (2)0.026 (2)−0.011 (2)
C20.050 (2)0.054 (2)0.069 (3)0.0123 (19)0.0077 (18)0.001 (2)
C40.054 (2)0.047 (2)0.056 (2)0.0082 (18)−0.0080 (18)0.0097 (18)
C80.064 (3)0.048 (2)0.064 (3)−0.0072 (19)0.017 (2)−0.0005 (19)
C60.052 (2)0.043 (2)0.048 (2)0.0008 (17)0.0005 (16)0.0045 (17)
C100.056 (3)0.060 (3)0.079 (3)−0.005 (2)0.022 (2)−0.021 (2)
C160.079 (3)0.060 (3)0.054 (2)−0.002 (2)−0.014 (2)0.014 (2)
C150.062 (3)0.055 (2)0.066 (3)0.010 (2)−0.014 (2)0.010 (2)
C30.050 (2)0.053 (2)0.073 (3)0.0150 (18)−0.003 (2)0.005 (2)
C180.062 (2)0.048 (2)0.044 (2)0.0049 (18)−0.0006 (17)−0.0006 (17)
C120.046 (2)0.0369 (18)0.057 (2)−0.0031 (16)0.0029 (16)−0.0060 (17)
C10.054 (2)0.059 (2)0.050 (2)0.0104 (19)0.0058 (17)0.0071 (18)
C110.052 (2)0.050 (2)0.072 (3)0.0041 (18)0.007 (2)−0.012 (2)
C130.043 (2)0.045 (2)0.064 (2)0.0045 (17)−0.0071 (17)0.0008 (18)
C70.048 (2)0.041 (2)0.052 (2)−0.0008 (15)0.0109 (16)−0.0039 (15)
C50.0442 (19)0.0398 (19)0.0458 (19)−0.0010 (15)−0.0032 (15)0.0020 (15)
Geometric parameters (Å, °) top
Mn1—N21.934 (3)C14—C151.379 (5)
Mn1—N31.937 (3)C14—C131.493 (6)
Mn1—N12.056 (3)C9—C101.387 (6)
Mn1—N42.070 (3)C9—C81.390 (6)
Mn1—N52.161 (3)C9—H9A0.9300
Mn1—O32.354 (3)C2—C31.369 (6)
N1—C11.341 (5)C2—C11.380 (5)
N1—C51.353 (4)C2—H2A0.9300
N2—C61.352 (5)C4—C31.380 (6)
N2—C71.414 (5)C4—C51.380 (5)
N3—C131.345 (5)C4—H4A0.9300
N3—C121.417 (5)C8—C71.392 (5)
N4—C181.336 (5)C8—H8A0.9300
N4—C141.348 (5)C6—C51.496 (5)
N5—N61.143 (4)C10—C111.371 (6)
N6—N71.174 (5)C10—H10A0.9300
O1—C61.222 (4)C16—C151.382 (6)
O2—C131.239 (4)C16—H16A0.9300
O3—C191.451 (5)C15—H15A0.9300
O3—H0.849 (10)C3—H3A0.9300
C19—H19A0.9600C18—H18A0.9300
C19—H19B0.9600C12—C111.389 (5)
C19—H19C0.9600C12—C71.408 (5)
C17—C161.374 (6)C1—H1A0.9300
C17—C181.380 (5)C11—H11A0.9300
C17—H17A0.9300
N2—Mn1—N381.55 (13)C8—C9—H9A119.8
N2—Mn1—N180.87 (12)C3—C2—C1119.2 (4)
N3—Mn1—N1161.63 (13)C3—C2—H2A120.4
N2—Mn1—N4161.93 (12)C1—C2—H2A120.4
N3—Mn1—N480.85 (12)C3—C4—C5118.8 (4)
N1—Mn1—N4116.19 (12)C3—C4—H4A120.6
N2—Mn1—N598.16 (13)C5—C4—H4A120.6
N3—Mn1—N598.81 (13)C9—C8—C7119.4 (4)
N1—Mn1—N588.92 (13)C9—C8—H8A120.3
N4—Mn1—N588.53 (12)C7—C8—H8A120.3
N2—Mn1—O394.67 (13)O1—C6—N2127.4 (4)
N3—Mn1—O394.08 (12)O1—C6—C5120.8 (3)
N1—Mn1—O382.11 (11)N2—C6—C5111.8 (3)
N4—Mn1—O382.57 (11)C11—C10—C9120.6 (4)
N5—Mn1—O3162.99 (13)C11—C10—H10A119.7
C1—N1—C5118.7 (3)C9—C10—H10A119.7
C1—N1—Mn1129.0 (2)C17—C16—C15119.2 (4)
C5—N1—Mn1112.3 (2)C17—C16—H16A120.4
C6—N2—C7125.6 (3)C15—C16—H16A120.4
C6—N2—Mn1118.4 (2)C14—C15—C16118.8 (4)
C7—N2—Mn1115.8 (2)C14—C15—H15A120.6
C13—N3—C12125.4 (3)C16—C15—H15A120.6
C13—N3—Mn1118.5 (3)C2—C3—C4119.6 (4)
C12—N3—Mn1116.0 (2)C2—C3—H3A120.2
C18—N4—C14118.8 (3)C4—C3—H3A120.2
C18—N4—Mn1129.4 (3)N4—C18—C17122.1 (4)
C14—N4—Mn1111.5 (2)N4—C18—H18A119.0
N6—N5—Mn1120.6 (3)C17—C18—H18A119.0
N5—N6—N7178.3 (5)C11—C12—C7119.8 (4)
C19—O3—Mn1129.3 (3)C11—C12—N3127.2 (4)
C19—O3—H108 (5)C7—C12—N3112.9 (3)
Mn1—O3—H102 (4)N1—C1—C2122.0 (4)
O3—C19—H19A109.5N1—C1—H1A119.0
O3—C19—H19B109.5C2—C1—H1A119.0
H19A—C19—H19B109.5C10—C11—C12120.0 (4)
O3—C19—H19C109.5C10—C11—H11A120.0
H19A—C19—H19C109.5C12—C11—H11A120.0
H19B—C19—H19C109.5O2—C13—N3127.1 (4)
C16—C17—C18119.1 (4)O2—C13—C14120.5 (4)
C16—C17—H17A120.4N3—C13—C14112.3 (3)
C18—C17—H17A120.4C8—C7—C12119.8 (4)
N4—C14—C15122.0 (4)C8—C7—N2126.5 (4)
N4—C14—C13116.3 (3)C12—C7—N2113.7 (3)
C15—C14—C13121.7 (4)N1—C5—C4121.8 (3)
C10—C9—C8120.4 (4)N1—C5—C6115.8 (3)
C10—C9—H9A119.8C4—C5—C6122.4 (3)
N2—Mn1—N1—C1174.5 (3)C10—C9—C8—C7−1.2 (6)
N3—Mn1—N1—C1157.5 (4)C7—N2—C6—O1−4.0 (6)
N4—Mn1—N1—C10.8 (4)Mn1—N2—C6—O1171.2 (3)
N5—Mn1—N1—C1−87.1 (3)C7—N2—C6—C5175.3 (3)
O3—Mn1—N1—C178.4 (3)Mn1—N2—C6—C5−9.6 (4)
N2—Mn1—N1—C5−5.0 (2)C8—C9—C10—C110.3 (6)
N3—Mn1—N1—C5−22.0 (5)C18—C17—C16—C15−0.3 (6)
N4—Mn1—N1—C5−178.7 (2)N4—C14—C15—C16−0.2 (6)
N5—Mn1—N1—C593.5 (2)C13—C14—C15—C16−178.2 (4)
O3—Mn1—N1—C5−101.0 (2)C17—C16—C15—C140.2 (6)
N3—Mn1—N2—C6−177.0 (3)C1—C2—C3—C40.6 (6)
N1—Mn1—N2—C68.3 (3)C5—C4—C3—C20.0 (6)
N4—Mn1—N2—C6169.9 (3)C14—N4—C18—C17−0.3 (6)
N5—Mn1—N2—C6−79.3 (3)Mn1—N4—C18—C17−173.8 (3)
O3—Mn1—N2—C689.5 (3)C16—C17—C18—N40.4 (6)
N3—Mn1—N2—C7−1.4 (3)C13—N3—C12—C113.5 (6)
N1—Mn1—N2—C7−176.1 (3)Mn1—N3—C12—C11−179.5 (3)
N4—Mn1—N2—C7−14.5 (6)C13—N3—C12—C7−178.3 (3)
N5—Mn1—N2—C796.4 (3)Mn1—N3—C12—C7−1.4 (4)
O3—Mn1—N2—C7−94.9 (3)C5—N1—C1—C20.8 (6)
N2—Mn1—N3—C13178.7 (3)Mn1—N1—C1—C2−178.6 (3)
N1—Mn1—N3—C13−164.4 (3)C3—C2—C1—N1−1.0 (6)
N4—Mn1—N3—C13−5.4 (3)C9—C10—C11—C120.6 (6)
N5—Mn1—N3—C1381.7 (3)C7—C12—C11—C10−0.6 (6)
O3—Mn1—N3—C13−87.2 (3)N3—C12—C11—C10177.5 (4)
N2—Mn1—N3—C121.5 (3)C12—N3—C13—O21.6 (6)
N1—Mn1—N3—C1218.5 (5)Mn1—N3—C13—O2−175.3 (3)
N4—Mn1—N3—C12177.5 (3)C12—N3—C13—C14179.9 (3)
N5—Mn1—N3—C12−95.5 (3)Mn1—N3—C13—C143.1 (4)
O3—Mn1—N3—C1295.7 (3)N4—C14—C13—O2−178.5 (3)
N2—Mn1—N4—C18−166.4 (4)C15—C14—C13—O2−0.4 (6)
N3—Mn1—N4—C18−179.5 (3)N4—C14—C13—N33.0 (5)
N1—Mn1—N4—C18−6.7 (4)C15—C14—C13—N3−178.8 (3)
N5—Mn1—N4—C1881.3 (3)C9—C8—C7—C121.2 (6)
O3—Mn1—N4—C18−84.1 (3)C9—C8—C7—N2−177.5 (4)
N2—Mn1—N4—C1419.8 (5)C11—C12—C7—C8−0.3 (5)
N3—Mn1—N4—C146.7 (2)N3—C12—C7—C8−178.6 (3)
N1—Mn1—N4—C14179.4 (2)C11—C12—C7—N2178.5 (3)
N5—Mn1—N4—C14−92.5 (3)N3—C12—C7—N20.2 (4)
O3—Mn1—N4—C14102.1 (3)C6—N2—C7—C8−4.9 (6)
N2—Mn1—N5—N6−85.4 (3)Mn1—N2—C7—C8179.8 (3)
N3—Mn1—N5—N6−2.8 (3)C6—N2—C7—C12176.3 (3)
N1—Mn1—N5—N6−166.0 (3)Mn1—N2—C7—C121.1 (4)
N4—Mn1—N5—N677.7 (3)C1—N1—C5—C4−0.2 (5)
O3—Mn1—N5—N6136.0 (4)Mn1—N1—C5—C4179.3 (3)
N2—Mn1—O3—C19−39.4 (4)C1—N1—C5—C6−178.1 (3)
N3—Mn1—O3—C19−121.2 (4)Mn1—N1—C5—C61.4 (4)
N1—Mn1—O3—C1940.7 (4)C3—C4—C5—N1−0.3 (6)
N4—Mn1—O3—C19158.6 (4)C3—C4—C5—C6177.5 (4)
N5—Mn1—O3—C1999.5 (5)O1—C6—C5—N1−175.8 (3)
C18—N4—C14—C150.3 (6)N2—C6—C5—N14.9 (5)
Mn1—N4—C14—C15174.8 (3)O1—C6—C5—C46.3 (6)
C18—N4—C14—C13178.4 (3)N2—C6—C5—C4−173.0 (3)
Mn1—N4—C14—C13−7.1 (4)
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O3—H···O2i0.849 (10)1.88 (2)2.696 (4)162 (6)
Symmetry codes: (i) −x, −y+1, −z.
Table 1
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O3—H···O2i0.849 (10)1.88 (2)2.696 (4)162 (6)
Symmetry codes: (i) −x, −y+1, −z.
Acknowledgements top

This work was supported by the National Natural Science Foundation of China (20471031, 20631030) and the National Basic Research Program of China (973 Program, 2007CB815305).

references
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