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The title compound, [MnN(C28H22N2O2)], has a distorted square-pyramidal coordination with an Mn[triple bond]N bond length of 1.516 (2) Å at the apical position. The five-membered chelate ring adopts a gauche conformation with the two phenyl groups in equatorial orientations.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100004492/qa0256sup1.cif
Contains datablocks mnrac, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100004492/qa0256Isup2.hkl
Contains datablock I

CCDC reference: 145632

Comment top

The crystal structure of [MnN{sal-(SS)-stien}].CH3CN was reported by Chang et al. (1998). We report here the crystal structure of [MnN(sal-rac-stien)], (I).

Experimental top

The title compound, [MnN(sal-rac-stien)], was prepared under aerobic conditions by the reaction of the chloromanganese(III) complex [MnCl(sal-rac-stien)] with NH4OH (15 equivalents) and NaOCl (6 equivalents). Crystals were grown from an acetonitorile solution.

Refinement top

All H-atom positional parameters were calculated geometrically and fixed with Uiso(H) = 1.2Ueq(parent atom).

Structure description top

The crystal structure of [MnN{sal-(SS)-stien}].CH3CN was reported by Chang et al. (1998). We report here the crystal structure of [MnN(sal-rac-stien)], (I).

Computing details top

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: TEXSAN.

(I) top
Crystal data top
[MnN(C28H22N2O2)]Z = 2
Mr = 487.44Dx = 1.412 Mg m3
Triclinic, P1Mo Kα radiation, λ = 0.71073 Å
a = 10.124 (4) ÅCell parameters from 25 reflections
b = 12.672 (3) Åθ = 14.7–15.0°
c = 9.632 (2) ŵ = 0.61 mm1
α = 110.83 (2)°T = 298 K
β = 96.36 (3)°Prismatic, green
γ = 85.32 (3)°0.7 × 0.2 × 0.2 mm
V = 1146.6 (6) Å3
Data collection top
Rigaku AFC-7R
diffractometer
Rint = 0.007
θ–2θ scansθmax = 27.5°, θmin = 2.5°
Absorption correction: ψ -scan
(North et al., 1968)
h = 130
Tmin = 0.824, Tmax = 0.886k = 1616
5556 measured reflectionsl = 1212
5258 independent reflections3 standard reflections every 150 reflections
4696 reflections with I > 2σ(I) intensity decay: none
Refinement top
Refinement on F2H-atom parameters not refined
R[F2 > 2σ(F2)] = 0.033 w = 1/[σ2(Fo2) + (0.0441P)2 + 0.5302P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.090(Δ/σ)max = 0.001
S = 1.04Δρmax = 0.46 e Å3
4696 reflectionsΔρmin = 0.25 e Å3
307 parameters
Crystal data top
[MnN(C28H22N2O2)]γ = 85.32 (3)°
Mr = 487.44V = 1146.6 (6) Å3
Triclinic, P1Z = 2
a = 10.124 (4) ÅMo Kα radiation
b = 12.672 (3) ŵ = 0.61 mm1
c = 9.632 (2) ÅT = 298 K
α = 110.83 (2)°0.7 × 0.2 × 0.2 mm
β = 96.36 (3)°
Data collection top
Rigaku AFC-7R
diffractometer
4696 reflections with I > 2σ(I)
Absorption correction: ψ -scan
(North et al., 1968)
Rint = 0.007
Tmin = 0.824, Tmax = 0.8863 standard reflections every 150 reflections
5556 measured reflections intensity decay: none
5258 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.033307 parameters
wR(F2) = 0.090H-atom parameters not refined
S = 1.04Δρmax = 0.46 e Å3
4696 reflectionsΔρmin = 0.25 e Å3
Special details top

Refinement. Refinement using reflections with F2 > 0.0 σ(F2). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mn10.58217 (2)0.12257 (2)0.41378 (3)0.03129 (8)
O20.6547 (1)0.0286 (1)0.3364 (1)0.0408 (3)
O30.7207 (1)0.1331 (1)0.5688 (1)0.0441 (3)
N40.4083 (1)0.0768 (1)0.3059 (2)0.0332 (3)
N50.4718 (1)0.2363 (1)0.5534 (2)0.0358 (3)
N60.6269 (2)0.1892 (1)0.3255 (2)0.0440 (3)
C70.6124 (2)0.1064 (1)0.2100 (2)0.0349 (3)
C80.7010 (2)0.1973 (2)0.1415 (2)0.0422 (4)
C90.6607 (2)0.2835 (2)0.0116 (2)0.0469 (4)
C100.5315 (2)0.2840 (2)0.0549 (2)0.0498 (4)
C110.4431 (2)0.1967 (2)0.0096 (2)0.0450 (4)
C120.4813 (2)0.1066 (1)0.1408 (2)0.0362 (3)
C130.3841 (2)0.0168 (1)0.1988 (2)0.0378 (3)
C140.7464 (2)0.2245 (1)0.6848 (2)0.0402 (4)
C150.8759 (2)0.2346 (2)0.7591 (3)0.0567 (5)
C160.9068 (2)0.3278 (2)0.8830 (3)0.0661 (6)
C170.8124 (3)0.4139 (2)0.9404 (3)0.0647 (6)
C180.6854 (2)0.4055 (2)0.8722 (2)0.0544 (5)
C190.6505 (2)0.3119 (1)0.7429 (2)0.0406 (4)
C200.5152 (2)0.3075 (2)0.6803 (2)0.0417 (4)
C210.3064 (2)0.1722 (1)0.3405 (2)0.0363 (3)
C220.1637 (2)0.1395 (1)0.2905 (2)0.0351 (3)
C230.0986 (2)0.1662 (2)0.1725 (2)0.0460 (4)
C240.0325 (2)0.1372 (2)0.1232 (2)0.0563 (5)
C250.0984 (2)0.0829 (2)0.1923 (3)0.0528 (5)
C260.0358 (2)0.0568 (2)0.3102 (3)0.0538 (5)
C270.0951 (2)0.0835 (2)0.3587 (2)0.0480 (4)
C280.3263 (2)0.2389 (1)0.5079 (2)0.0386 (3)
C290.2652 (2)0.3582 (2)0.5438 (2)0.0443 (4)
C300.3196 (3)0.4359 (2)0.4974 (3)0.0684 (6)
C310.2670 (4)0.5445 (2)0.5327 (4)0.0931 (10)
C320.1600 (4)0.5777 (2)0.6123 (4)0.097 (1)
C330.1017 (3)0.5034 (3)0.6597 (3)0.092 (1)
C340.1555 (2)0.3907 (2)0.6245 (2)0.0619 (6)
H80.79130.19900.18630.0496*
H90.72300.34490.03310.0554*
H100.50260.34440.14530.0589*
H110.35270.19720.03570.0522*
H130.29340.02740.15560.0441*
H150.94330.17410.72510.0660*
H160.99820.33390.93020.0775*
H170.83490.47811.02880.0780*
H180.61930.46530.91250.0634*
H200.45210.36230.73740.0482*
H210.32820.22200.29030.0412*
H230.14520.20700.12540.0537*
H240.07700.15500.04080.0658*
H250.18850.06340.15700.0612*
H260.08400.01890.35820.0631*
H270.13920.06490.44260.0565*
H280.28100.20070.55820.0440*
H300.39560.41240.43550.0792*
H310.30620.59980.50050.1112*
H320.12290.65570.63360.1070*
H330.02320.52640.71430.1081*
H340.11790.33910.66030.0741*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0291 (1)0.0290 (1)0.0340 (1)0.00191 (8)0.00296 (9)0.00871 (9)
O20.0359 (6)0.0328 (6)0.0457 (7)0.0011 (5)0.0023 (5)0.0063 (5)
O30.0406 (6)0.0358 (6)0.0463 (7)0.0001 (5)0.0075 (5)0.0065 (5)
N40.0295 (6)0.0311 (6)0.0372 (7)0.0008 (5)0.0050 (5)0.0093 (5)
N50.0335 (7)0.0333 (7)0.0377 (7)0.0011 (5)0.0034 (5)0.0089 (6)
N60.0405 (8)0.0455 (8)0.0492 (8)0.0047 (6)0.0091 (6)0.0184 (7)
C70.0373 (8)0.0295 (7)0.0378 (8)0.0010 (6)0.0072 (6)0.0105 (6)
C80.0391 (9)0.0367 (8)0.0488 (10)0.0030 (7)0.0088 (7)0.0122 (7)
C90.054 (1)0.0340 (8)0.0489 (10)0.0063 (7)0.0172 (8)0.0077 (7)
C100.063 (1)0.0394 (9)0.0377 (9)0.0001 (8)0.0067 (8)0.0018 (7)
C110.0470 (10)0.0411 (9)0.0388 (9)0.0008 (7)0.0011 (7)0.0059 (7)
C120.0383 (8)0.0323 (8)0.0349 (8)0.0010 (6)0.0043 (6)0.0079 (6)
C130.0317 (8)0.0366 (8)0.0403 (8)0.0019 (6)0.0001 (6)0.0087 (7)
C140.0440 (9)0.0356 (8)0.0403 (9)0.0080 (7)0.0048 (7)0.0138 (7)
C150.051 (1)0.046 (1)0.063 (1)0.0038 (9)0.0160 (9)0.0127 (9)
C160.062 (1)0.056 (1)0.068 (1)0.012 (1)0.027 (1)0.014 (1)
C170.078 (2)0.048 (1)0.053 (1)0.016 (1)0.019 (1)0.0041 (9)
C180.064 (1)0.0422 (10)0.046 (1)0.0064 (9)0.0035 (9)0.0025 (8)
C190.0468 (9)0.0360 (8)0.0368 (8)0.0091 (7)0.0011 (7)0.0096 (7)
C200.0428 (9)0.0373 (8)0.0392 (9)0.0020 (7)0.0072 (7)0.0052 (7)
C210.0322 (8)0.0333 (8)0.0431 (9)0.0004 (6)0.0052 (6)0.0126 (7)
C220.0282 (7)0.0309 (7)0.0428 (8)0.0011 (6)0.0063 (6)0.0082 (6)
C230.0436 (9)0.050 (1)0.0468 (10)0.0023 (8)0.0072 (8)0.0194 (8)
C240.045 (1)0.067 (1)0.053 (1)0.0046 (9)0.0048 (9)0.021 (1)
C250.0292 (8)0.053 (1)0.064 (1)0.0003 (8)0.0060 (8)0.0056 (9)
C260.0427 (10)0.053 (1)0.068 (1)0.0095 (8)0.0157 (9)0.0188 (10)
C270.0452 (10)0.049 (1)0.056 (1)0.0071 (8)0.0026 (8)0.0249 (9)
C280.0350 (8)0.0362 (8)0.0425 (9)0.0002 (6)0.0073 (7)0.0104 (7)
C290.0427 (9)0.0362 (9)0.0450 (9)0.0043 (7)0.0019 (7)0.0047 (7)
C300.076 (2)0.041 (1)0.087 (2)0.004 (1)0.009 (1)0.020 (1)
C310.123 (3)0.040 (1)0.107 (2)0.001 (1)0.006 (2)0.018 (1)
C320.129 (3)0.047 (1)0.086 (2)0.030 (2)0.016 (2)0.003 (1)
C330.076 (2)0.109 (2)0.055 (1)0.049 (2)0.006 (1)0.002 (1)
C340.054 (1)0.075 (1)0.048 (1)0.019 (1)0.0091 (9)0.014 (1)
Geometric parameters (Å, º) top
Mn1—O21.908 (1)C18—C191.415 (2)
Mn1—O31.908 (1)C18—H180.969
Mn1—N41.962 (1)C19—C201.431 (3)
Mn1—N51.956 (1)C20—H200.962
Mn1—N61.516 (2)C21—C221.514 (2)
O2—C71.318 (2)C21—C281.530 (2)
O3—C141.312 (2)C21—H210.972
N4—C131.285 (2)C22—C231.382 (3)
N4—C211.491 (2)C22—C271.390 (3)
N5—C201.290 (2)C23—C241.392 (3)
N5—C281.490 (2)C23—H230.974
C7—C81.410 (2)C24—C251.364 (4)
C7—C121.417 (2)C24—H240.957
C8—C91.383 (2)C25—C261.368 (4)
C8—H80.968C25—H250.958
C9—C101.390 (3)C26—C271.383 (3)
C9—H90.965C26—H260.964
C10—C111.373 (3)C27—H270.973
C10—H100.968C28—C291.520 (3)
C11—C121.410 (2)C28—H280.965
C11—H110.969C29—C301.388 (4)
C12—C131.437 (2)C29—C341.378 (3)
C13—H130.964C30—C311.372 (4)
C14—C151.415 (3)C30—H300.987
C14—C191.410 (2)C31—C321.349 (6)
C15—C161.376 (3)C31—H310.986
C15—H150.973C32—C331.378 (6)
C16—C171.388 (3)C32—H320.987
C16—H160.981C33—C341.421 (4)
C17—C181.372 (3)C33—H330.969
C17—H170.966C34—H340.960
O2—Mn1—O382.15 (5)C14—C19—C18119.8 (2)
O2—Mn1—N491.34 (5)C14—C19—C20122.4 (1)
O2—Mn1—N5149.84 (7)C18—C19—C20117.8 (2)
O2—Mn1—N6108.56 (7)N5—C20—C19125.0 (2)
O3—Mn1—N4154.34 (7)N5—C20—H20117.7
O3—Mn1—N591.06 (6)C19—C20—H20117.2
O3—Mn1—N6105.47 (7)N4—C21—C22115.6 (1)
N4—Mn1—N582.16 (6)N4—C21—C28107.4 (1)
N4—Mn1—N6100.14 (8)N4—C21—H21106.5
N5—Mn1—N6101.58 (7)C22—C21—C28112.2 (1)
Mn1—O2—C7125.6 (1)C22—C21—H21108.1
Mn1—O3—C14125.0 (1)C28—C21—H21106.4
Mn1—N4—C13126.3 (1)C21—C22—C23119.1 (2)
Mn1—N4—C21112.19 (9)C21—C22—C27122.5 (2)
C13—N4—C21120.5 (1)C23—C22—C27118.4 (2)
Mn1—N5—C20125.1 (1)C22—C23—C24120.6 (2)
Mn1—N5—C28116.51 (9)C22—C23—H23119.0
C20—N5—C28118.4 (1)C24—C23—H23120.3
O2—C7—C8118.3 (1)C23—C24—C25120.0 (2)
O2—C7—C12124.0 (1)C23—C24—H24120.4
C8—C7—C12117.7 (1)C25—C24—H24119.6
C7—C8—C9120.9 (2)C24—C25—C26120.1 (2)
C7—C8—H8119.3C24—C25—H25119.0
C9—C8—H8119.8C26—C25—H25120.9
C8—C9—C10121.3 (2)C25—C26—C27120.5 (2)
C8—C9—H9119.4C25—C26—H26119.0
C10—C9—H9119.3C27—C26—H26120.5
C9—C10—C11119.0 (2)C22—C27—C26120.3 (2)
C9—C10—H10121.6C22—C27—H27119.4
C11—C10—H10119.4C26—C27—H27120.2
C10—C11—C12121.2 (2)N5—C28—C21107.7 (1)
C10—C11—H11119.3N5—C28—C29112.9 (1)
C12—C11—H11119.4N5—C28—H28109.6
C7—C12—C11119.9 (1)C21—C28—C29110.8 (2)
C7—C12—C13122.3 (1)C21—C28—H28107.4
C11—C12—C13117.8 (2)C29—C28—H28108.4
N4—C13—C12124.9 (1)C28—C29—C30120.7 (2)
N4—C13—H13117.1C28—C29—C34120.0 (2)
C12—C13—H13118.0C30—C29—C34119.2 (2)
O3—C14—C15118.5 (2)C29—C30—C31121.0 (3)
O3—C14—C19123.5 (2)C29—C30—H30119.8
C15—C14—C19117.9 (1)C31—C30—H30119.1
C14—C15—C16120.7 (2)C30—C31—C32120.4 (3)
C14—C15—H15120.1C30—C31—H31121.0
C16—C15—H15119.2C32—C31—H31118.6
C15—C16—C17121.5 (2)C31—C32—C33120.7 (3)
C15—C16—H16118.9C31—C32—H32118.5
C17—C16—H16119.6C33—C32—H32120.8
C16—C17—C18119.2 (2)C32—C33—C34119.5 (3)
C16—C17—H17120.6C32—C33—H33120.9
C18—C17—H17120.2C34—C33—H33119.6
C17—C18—C19121.0 (2)C29—C34—C33119.1 (3)
C17—C18—H18119.2C29—C34—H34120.6
C19—C18—H18119.8C33—C34—H34120.2

Experimental details

Crystal data
Chemical formula[MnN(C28H22N2O2)]
Mr487.44
Crystal system, space groupTriclinic, P1
Temperature (K)298
a, b, c (Å)10.124 (4), 12.672 (3), 9.632 (2)
α, β, γ (°)110.83 (2), 96.36 (3), 85.32 (3)
V3)1146.6 (6)
Z2
Radiation typeMo Kα
µ (mm1)0.61
Crystal size (mm)0.7 × 0.2 × 0.2
Data collection
DiffractometerRigaku AFC-7R
Absorption correctionψ -scan
(North et al., 1968)
Tmin, Tmax0.824, 0.886
No. of measured, independent and
observed [I > 2σ(I)] reflections
5556, 5258, 4696
Rint0.007
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.033, 0.090, 1.04
No. of reflections4696
No. of parameters307
No. of restraints?
H-atom treatmentH-atom parameters not refined
Δρmax, Δρmin (e Å3)0.46, 0.25

Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation, 1999), SIR92 (Altomare et al., 1994), SHELXL97 (Sheldrick, 1997), TEXSAN.

Selected bond lengths (Å) top
Mn1—O21.908 (1)Mn1—N51.956 (1)
Mn1—O31.908 (1)Mn1—N61.516 (2)
Mn1—N41.962 (1)
 

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