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The title compound, aquachloro{2,2′-[1,2-ethanediylbis(nitrilomethylidyne)]diphenolato-κ
4O,
N,
N′,
O′}manganese(III),[MnCl(C
16H
14N
2O
2)(H
2O)], is a neutral manganese(III) complex with a pseudo-octahedral metal centre. The equatorial plane comprises the four donor atoms of the tetradentate Schiff base ligand [Mn—O 1.886 (4) and 1.893 (4) Å, and Mn—N 1.978 (5) and 1.982 (5) Å], with a water molecule [Mn—O 2.383 (4) Å] and a Cl
− ligand [Mn—Cl 2.4680 (16) Å] completing the coordination sphere. The distorted geometry is highlighted by the marked displacement of the Mn
III ion out of the least-squares plane of the four Schiff base donor atoms by 0.165 (2) Å. These monomeric Mn
III centres are then linked into a polymeric array
via hydrogen bonds between the coordinated water molecule and the phenolic O-atom donors of an adjacent Mn
III centre [O—H
O 2.789 (5) and 2.881 (5) Å].
Supporting information
CCDC reference: 184479
Data collection: CAD-4-PC Software (Enraf Nonius, 1994); cell refinement: CAD-4-PC Software; data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and PLUTON in PLATON (Spek, 1998); software used to prepare material for publication: WinGX (Farrugia, 1999).
Aquachloro{2,2'-[1,2-ethanediylbis(nitrilomethylidyne)]diphenolato-
κ4O,
N,
N',
O'}manganese(III)
top
Crystal data top
[MnCl(C16H14N2O2)(H2O)] | F(000) = 384 |
Mr = 374.7 | Dx = 1.6 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P2yb | Cell parameters from 25 reflections |
a = 10.418 (4) Å | θ = 8.1–13.9° |
b = 6.627 (3) Å | µ = 1.04 mm−1 |
c = 11.733 (5) Å | T = 160 K |
β = 106.29 (2)° | Prism, brown |
V = 777.5 (6) Å3 | 0.3 × 0.2 × 0.1 mm |
Z = 2 | |
Data collection top
Enraf Nonius CAD-4 diffractometer | Rint = 0.030 |
non–profiled ω/2θ scans | θmax = 25.0°, θmin = 1.8° |
Absorption correction: ψ scan (North et al., 1968) | h = −12→11 |
Tmin = 0.675, Tmax = 0.902 | k = 0→7 |
1562 measured reflections | l = 0→13 |
1488 independent reflections | 2 standard reflections every 60 min |
1324 reflections with I > 2σ(I) | intensity decay: none |
Refinement top
Refinement on F2 | H atoms treated by a mixture of independent and constrained refinement |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.072P)2 + 0.0385P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.037 | (Δ/σ)max < 0.001 |
wR(F2) = 0.099 | Δρmax = 0.44 e Å−3 |
S = 1.04 | Δρmin = −0.60 e Å−3 |
1488 reflections | Absolute structure: Flack (1983) |
184 parameters | Absolute structure parameter: 0.01 (4) |
1 restraint | |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mn1 | 0.33140 (7) | 0.87645 (12) | 0.11213 (6) | 0.0154 (2) | |
Cl1 | 0.19336 (12) | 0.9867 (2) | 0.24060 (11) | 0.0227 (3) | |
O1 | 0.4891 (3) | 1.0167 (6) | 0.1925 (3) | 0.0186 (8) | |
O2 | 0.2789 (3) | 1.0717 (6) | −0.0090 (3) | 0.0188 (8) | |
O3 | 0.4607 (3) | 0.7364 (7) | −0.0068 (3) | 0.0264 (10) | |
H16 | 0.539 | 0.7141 | 0.0265 | 0.06* | |
H17 | 0.4551 | 0.6665 | −0.0654 | 0.06* | |
N1 | 0.3900 (4) | 0.6378 (7) | 0.2148 (4) | 0.0164 (9) | |
N2 | 0.1926 (4) | 0.6858 (8) | 0.0235 (4) | 0.0196 (10) | |
C1 | 0.5605 (3) | 0.9895 (6) | 0.3075 (2) | 0.0170 (11) | |
C2 | 0.6450 (3) | 1.1458 (5) | 0.3610 (3) | 0.0255 (13) | |
H2 | 0.648 | 1.2666 | 0.3182 | 0.031* | |
C3 | 0.7251 (3) | 1.1253 (5) | 0.4771 (3) | 0.0301 (15) | |
H3 | 0.7829 | 1.2321 | 0.5136 | 0.036* | |
C4 | 0.7207 (3) | 0.9486 (6) | 0.5396 (2) | 0.0305 (15) | |
H4 | 0.7754 | 0.9346 | 0.619 | 0.037* | |
C5 | 0.6362 (4) | 0.7923 (5) | 0.4861 (3) | 0.0261 (13) | |
H5 | 0.6331 | 0.6715 | 0.5289 | 0.031* | |
C6 | 0.5561 (3) | 0.8127 (5) | 0.3700 (3) | 0.0221 (13) | |
C7 | 0.4779 (5) | 0.6391 (9) | 0.3174 (4) | 0.0192 (12) | |
H7 | 0.4922 | 0.5168 | 0.3614 | 0.023* | |
C8 | 0.3216 (6) | 0.4511 (9) | 0.1660 (5) | 0.0238 (13) | |
H8A | 0.3197 | 0.3563 | 0.2307 | 0.029* | |
H8B | 0.3679 | 0.3852 | 0.1129 | 0.029* | |
C9 | 0.1800 (5) | 0.5112 (9) | 0.0968 (5) | 0.0238 (12) | |
H9A | 0.1348 | 0.3982 | 0.046 | 0.029* | |
H9B | 0.127 | 0.5474 | 0.1519 | 0.029* | |
C10 | 0.1247 (5) | 0.6997 (9) | −0.0861 (5) | 0.0224 (13) | |
H10 | 0.0641 | 0.5937 | −0.1189 | 0.027* | |
C11 | 0.1348 (3) | 0.8677 (5) | −0.1631 (3) | 0.0217 (11) | |
C12 | 0.0649 (3) | 0.8474 (5) | −0.2822 (3) | 0.0270 (14) | |
H12 | 0.0157 | 0.7277 | −0.3095 | 0.032* | |
C13 | 0.0672 (4) | 1.0021 (7) | −0.3616 (2) | 0.0360 (16) | |
H13 | 0.0195 | 0.9882 | −0.4431 | 0.043* | |
C14 | 0.1393 (4) | 1.1772 (6) | −0.3218 (3) | 0.0328 (16) | |
H14 | 0.1408 | 1.283 | −0.3761 | 0.039* | |
C15 | 0.2091 (4) | 1.1976 (5) | −0.2026 (3) | 0.0274 (14) | |
H15 | 0.2584 | 1.3173 | −0.1754 | 0.033* | |
C16 | 0.2069 (3) | 1.0428 (6) | −0.1233 (2) | 0.0193 (12) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.0228 (4) | 0.0134 (4) | 0.0126 (4) | −0.0010 (4) | 0.0090 (3) | 0.0003 (4) |
Cl1 | 0.0283 (7) | 0.0235 (8) | 0.0213 (7) | 0.0040 (6) | 0.0150 (5) | −0.0020 (6) |
N1 | 0.027 (2) | 0.016 (2) | 0.011 (2) | −0.0003 (19) | 0.0146 (18) | −0.0013 (19) |
N2 | 0.024 (2) | 0.020 (3) | 0.019 (2) | 0.000 (2) | 0.0139 (19) | −0.002 (2) |
O1 | 0.0226 (17) | 0.019 (2) | 0.0148 (17) | −0.0018 (16) | 0.0063 (14) | 0.0000 (16) |
O2 | 0.0247 (18) | 0.020 (2) | 0.0116 (17) | −0.0044 (16) | 0.0054 (14) | −0.0013 (17) |
O3 | 0.028 (2) | 0.036 (3) | 0.0181 (19) | 0.0046 (19) | 0.0126 (17) | −0.0084 (19) |
C1 | 0.023 (2) | 0.022 (3) | 0.011 (2) | 0.000 (3) | 0.012 (2) | 0.001 (3) |
C2 | 0.028 (3) | 0.033 (4) | 0.016 (3) | 0.004 (3) | 0.008 (2) | −0.003 (3) |
C3 | 0.026 (3) | 0.038 (4) | 0.026 (3) | −0.001 (3) | 0.008 (2) | −0.011 (3) |
C4 | 0.029 (3) | 0.051 (5) | 0.016 (3) | 0.001 (3) | 0.014 (2) | −0.001 (3) |
C5 | 0.027 (3) | 0.044 (4) | 0.012 (3) | 0.008 (3) | 0.013 (2) | 0.010 (3) |
C6 | 0.021 (2) | 0.035 (4) | 0.015 (3) | 0.009 (2) | 0.013 (2) | −0.003 (2) |
C7 | 0.026 (3) | 0.018 (3) | 0.021 (3) | 0.005 (2) | 0.020 (2) | 0.004 (2) |
C8 | 0.041 (3) | 0.015 (3) | 0.021 (3) | −0.002 (2) | 0.017 (2) | −0.002 (2) |
C9 | 0.033 (3) | 0.016 (3) | 0.026 (3) | −0.005 (3) | 0.015 (2) | −0.004 (3) |
C10 | 0.019 (3) | 0.022 (3) | 0.029 (3) | −0.005 (2) | 0.011 (2) | −0.007 (3) |
C11 | 0.016 (2) | 0.036 (3) | 0.016 (2) | −0.001 (3) | 0.0087 (18) | −0.004 (3) |
C12 | 0.026 (3) | 0.036 (4) | 0.020 (3) | −0.003 (3) | 0.009 (2) | −0.006 (3) |
C13 | 0.030 (3) | 0.061 (5) | 0.017 (3) | −0.002 (3) | 0.006 (2) | −0.001 (3) |
C14 | 0.028 (3) | 0.053 (5) | 0.019 (3) | 0.003 (3) | 0.010 (2) | 0.011 (3) |
C15 | 0.023 (3) | 0.035 (4) | 0.025 (3) | −0.001 (3) | 0.008 (2) | 0.004 (3) |
C16 | 0.015 (2) | 0.032 (3) | 0.012 (2) | 0.006 (2) | 0.006 (2) | 0.004 (2) |
Geometric parameters (Å, º) top
Mn1—Cl1 | 2.4680 (16) | C5—C6 | 1.39 |
Mn1—O1 | 1.893 (4) | C5—H5 | 0.95 |
Mn1—O2 | 1.886 (4) | C6—C7 | 1.445 (6) |
Mn1—O3 | 2.383 (4) | C7—H7 | 0.95 |
Mn1—N1 | 1.978 (5) | C8—C9 | 1.524 (8) |
Mn1—N2 | 1.982 (5) | C8—H8A | 0.99 |
N1—C7 | 1.292 (6) | C8—H8B | 0.99 |
N1—C8 | 1.462 (7) | C9—H9A | 0.99 |
N2—C10 | 1.285 (7) | C9—H9B | 0.99 |
N2—C9 | 1.469 (7) | C10—C11 | 1.456 (7) |
O1—C1 | 1.358 (4) | C10—H10 | 0.95 |
O2—C16 | 1.354 (4) | C11—C12 | 1.39 |
O3—H16 | 0.814 | C11—C16 | 1.39 |
O3—H17 | 0.817 | C12—C13 | 1.39 |
C1—C2 | 1.39 | C12—H12 | 0.95 |
C1—C6 | 1.39 | C13—C14 | 1.39 |
C2—C3 | 1.39 | C13—H13 | 0.95 |
C2—H2 | 0.95 | C14—C15 | 1.39 |
C3—C4 | 1.39 | C14—H14 | 0.95 |
C3—H3 | 0.95 | C15—C16 | 1.39 |
C4—C5 | 1.39 | C15—H15 | 0.95 |
C4—H4 | 0.95 | | |
| | | |
O1—Mn1—O2 | 93.78 (16) | C5—C6—C1 | 120 |
O1—Mn1—O3 | 85.92 (15) | C5—C6—C7 | 116.9 (3) |
O2—Mn1—O3 | 85.29 (16) | C1—C6—C7 | 122.9 (3) |
O1—Mn1—N1 | 90.74 (17) | N1—C7—C6 | 124.8 (5) |
O1—Mn1—N2 | 168.06 (18) | N1—C7—H7 | 117.6 |
O2—Mn1—N1 | 169.17 (17) | C6—C7—H7 | 117.6 |
O2—Mn1—N2 | 91.58 (17) | N1—C8—C9 | 106.3 (5) |
O3—Mn1—N1 | 85.22 (16) | N1—C8—H8A | 110.5 |
O3—Mn1—N2 | 83.89 (16) | C9—C8—H8A | 110.5 |
N1—Mn1—N2 | 82.2 (2) | N1—C8—H8B | 110.5 |
O1—Mn1—Cl1 | 97.08 (12) | C9—C8—H8B | 110.5 |
O2—Mn1—Cl1 | 99.30 (12) | H8A—C8—H8B | 108.7 |
O3—Mn1—Cl1 | 174.31 (12) | N2—C9—C8 | 106.6 (4) |
N1—Mn1—Cl1 | 89.89 (12) | N2—C9—H9A | 110.4 |
N2—Mn1—Cl1 | 92.57 (13) | C8—C9—H9A | 110.4 |
C7—N1—C8 | 120.7 (5) | N2—C9—H9B | 110.4 |
C7—N1—Mn1 | 125.4 (4) | C8—C9—H9B | 110.4 |
C8—N1—Mn1 | 113.9 (3) | H9A—C9—H9B | 108.6 |
C10—N2—C9 | 121.8 (5) | N2—C10—C11 | 124.1 (5) |
C10—N2—Mn1 | 126.5 (4) | N2—C10—H10 | 118 |
C9—N2—Mn1 | 111.5 (3) | C11—C10—H10 | 118 |
C1—O1—Mn1 | 125.9 (3) | C12—C11—C16 | 120 |
C16—O2—Mn1 | 127.7 (3) | C12—C11—C10 | 116.2 (3) |
H16—O3—H17 | 97.3 | C16—C11—C10 | 123.8 (3) |
O1—C1—C2 | 116.8 (3) | C13—C12—C11 | 120 |
O1—C1—C6 | 123.1 (3) | C13—C12—H12 | 120 |
C2—C1—C6 | 120 | C11—C12—H12 | 120 |
C3—C2—C1 | 120 | C14—C13—C12 | 120 |
C3—C2—H2 | 120 | C14—C13—H13 | 120 |
C1—C2—H2 | 120 | C12—C13—H13 | 120 |
C4—C3—C2 | 120 | C15—C14—C13 | 120 |
C4—C3—H3 | 120 | C15—C14—H14 | 120 |
C2—C3—H3 | 120 | C13—C14—H14 | 120 |
C3—C4—C5 | 120 | C16—C15—C14 | 120 |
C3—C4—H4 | 120 | C16—C15—H15 | 120 |
C5—C4—H4 | 120 | C14—C15—H15 | 120 |
C6—C5—C4 | 120 | O2—C16—C15 | 116.8 (3) |
C6—C5—H5 | 120 | O2—C16—C11 | 123.2 (3) |
C4—C5—H5 | 120 | C15—C16—C11 | 120 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H17···O1i | 0.82 | 2.01 | 2.789 (5) | 160 |
O3—H16···O2i | 0.81 | 2.18 | 2.881 (5) | 145 |
Symmetry code: (i) −x+1, y−1/2, −z. |
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