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Di μ sulfato κ3O,O′:O′′;κ3O,O′:O′′ bis­­{aqua­[2,4,6 tris­­(2 pyrid­yl) 1,3,5 triazine κ3N1,N2,N6]manganese(II)} tetra­hydrate

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metal-organic papers

Acta Cryst.(2006). E62, m141–m143 doi:10.1107/S1600536805041528 Dı´az de Vivaret al. [Mn

2(SO4)2(C16H12N6)2(H2O)2]4H2O

m141

Acta Crystallographica Section E

Structure Reports Online

ISSN 1600-5368

Di-

l

-sulfato-

j

3

O

,

O

000

:

O

000000

;

j

3

O

,

O

000

:

O

000000

-bis{aqua-[2,4,6-tris(2-pyridyl)-1,3,5-triazine-

j

3

N

1

,

N

2

,

N

6

]-manganese(II)} tetrahydrate

M. Enriqueta Dı´az de Vivar,a Sergio Baggio,aMarı´a Teresa Garlandband Ricardo Baggioc*

aUniversidad Nacional de la Patagonia, Sede

Puerto Madryn, 9120 Puerto Madryn, Chubut, Argentina, and CenPat, CONICET, 9120 Puerto Madryn, Chubut, Argentina,bFacultad de

Cien-cias Fı´sicas y Matema´ticas, Universidad de Chile and CIMAT, Casilla 487-3, Santiago de Chile, Chile, andcDepartamento de Fı´sica, Comisio´n Nacional de Energı´a Ato´mica, Buenos Aires, Argentina

Correspondence e-mail: baggio@cnea.gov.ar

Key indicators

Single-crystal X-ray study

T= 291 K

Mean(C–C) = 0.008 A˚

Rfactor = 0.066

wRfactor = 0.109

Data-to-parameter ratio = 12.7

For details of how these key indicators were automatically derived from the article, see http://journals.iucr.org/e.

#2006 International Union of Crystallography Printed in Great Britain – all rights reserved

The title compound, [Mn2(SO4)2(C16H12N6)2(H2O)2]4H2O, crystallizes as dimers built up around inversion centers. The Mn cation is seven-coordinated in the form of a pentagonal bipyramid, with three sulfate O atoms involved in its coordination (two equatorial and one axial). The sulfate species also bridge to the second Mn cation. The other three equatorial sites are occupied by N atoms from the tridentate 2,4,6-tris(2-pyridyl)-1,3,5-triazine ligand and the remaining axial site by a water molecule. This compound is isostructural with the previously reported Cd analog.

Comment

In the past few years we have reported a number of thiosulfate and sulfite complexes obtained by decomposition of less common sulfur oxoanions such as dithionite and pyrosulfite. The important aspect is the instability of these anions in aqueous solutions (Remy, 1956), which, when interacting with transition metal ions and organic ligands, can produce a wide variety of transformation products. The high instability, which makes the chemistry of these anions so difficult, makes them attractive as precursors. Some previously unintentional outcomes (Harveyet al., 2004) suggested, and further rational synthesis confirmed (Dı´az de Vivar et al., 2004), that the method could be an alternative route for the preparation of thiosulfate or sulfite complexes where direct synthesis had previously proven unsuccessful.

In spite of the achievements of the method in generating interesting structures, the fascinating reactions it promotes have usualy remained far beyond the chemist’s control and

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their outcomes have been, more often than not, mainly determined by chance. An example of this assertion is presented here,viz.the title compound, [Mn(SO4)(C16H12N6 )-(H2O)]24H2O, (I), a manganese sulfate complex serendipi-tously obtained when aiming for the thiosulfate analog.

Compound (I) is a dimeric centrosymmetric species isostructural to the Cd analog obtained by a conventional synthesis starting from a sulfate salt (Harvey et al., 2003). Compound (I) displays a seven-coordinate environment around the Mn ion, with three N atoms from a tridentate 2,4,6-tris(2-pyridyl)-1,3,5-triazine (tpt) molecule, one O atom from a water molecule and three further O atoms from each of two symmetry-related sulfate ions, each one of which binds to two metal centers, thus generating the dimeric structure (Fig. 1).

The coordination polyhedron about Mn can be described as a distorted pentagonal bipyramid, with the equatorial plane formed by atoms N1, N2, N3, O1 and O2 [maximum deviation from the mean plane = 0.04 (1) A˚ for N2] and equatorial angles subtended at the Mn site ranging from 60.49 (11) to 85.09 (12) (ideal 72). The axial sites are occupied by O1W and O4i[symmetry code: (i)x,y,z] and they subtend an angle of 167.75 (12)at the metal.

The S—O distances in the sulfate group are all similar (Table 1), suggesting double-bond delocalization. The mean value [1.461 (9) A˚ ] is similar to that reported for the free anion; a search in the November 2004 version of the Cambridge Structural Database (CSD; Allen, 2002) gave a mean value of 1.472 (8) A˚ for 118 structures withR< 0.05.

The tpt anion is almost planar and acts as a tridentate species, with its central Mn—N bond [2.257 (3) A˚ ] being significantly shorter than the lateral ones [2.376 (4) and 2.378 (4) A˚ ]. The ligand does not show any abnormal features,

with its three bound rings being almost coplanar: the atoms deviate, on average, from an ideal plane by less than 0.02 (1) A˚ . The terminal pyridyl ring deviates from planarity by less than 0.01 (1) A˚ and the dihedral angle it makes with the metal-bonded ring system is 3.6 (1).

As a result of the dimers being located around an inversion center, their planar tpt molecules are parallel to each other. Crystal symmetry preserves the orientation of the dimeric units, which stack in sets of parallel planes, alternately sharing one of the two layers in the double molecular units. This disposition (Fig. 2) results in a set of interleaved planar arrays at a nearly graphitic (ca 3.6 A˚ ) distance from one another. Thus, the molecules of (I) are linked by – interactions between aromatic rings (Table 3) as well as an extensive hydrogen-bonding network, having all the available water molecules as donors and some water O atoms, tpt N atoms and some sulfate O atoms as acceptors (Table 2).

Experimental

A 96% ethanol solution of 2,20-dipyridylamine was diffused into an

aqueous solution containing MnCl24H2O, sodium dithionite and

potassium pyrosulfite (1:1:2 molar ratio). After two weeks a few colorless prisms of (I) suitable for X-ray analysis were obtained.

Crystal data

[Mn2(SO4)2(C16H12N6)2

-(H2O)2]4H2O

Mr= 1034.77 Triclinic,P1 a= 8.8737 (16) A˚ b= 10.5634 (19) A˚ c= 12.587 (2) A˚

= 103.566 (3) = 97.981 (3) = 110.409 (3)

V= 1042.9 (3) A˚3

Z= 1

Dx= 1.648 Mg m3

MoKradiation Cell parameters from 1017

reflections

= 5.1–43.9 = 0.79 mm1

T= 291 (2) K Prism, colorless 0.220.160.14 mm

metal-organic papers

m142

Dı´az de Vivaret al. [Mn

2(SO4)2(C16H12N6)2(H2O)2]4H2O Acta Cryst.(2006). E62, m141–m143

Figure 1

[image:2.610.312.564.68.260.2] [image:2.610.43.307.69.318.2]

View of (I), showing 50% displacement ellipsoids. [Symmetry code: (i) x,y,z.]

Figure 2

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Data collection

Bruker SMART CCD diffractometer

’and!scans

Absorption correction: multi-scan (SADABS; Sheldrick, 2001) Tmin= 0.846,Tmax= 0.898

8696 measured reflections

4041 independent reflections 2775 reflections withI> 2(I) Rint= 0.058

max= 26.0

h=10!10 k=13!12 l=16!15

Refinement

Refinement onF2

R[F2> 2(F2)] = 0.066

wR(F2) = 0.109

S= 1.05 4041 reflections 319 parameters

H atoms treated by a mixture of independent and constrained refinement

w= 1/[2(F

o2) + (0.013P)2

+ 2.08P]

whereP= (Fo2+ 2Fc2)/3

(/)max= 0.026

max= 0.46 e A˚ 3

min=0.39 e A˚ 3

Table 1

Selected interatomic distances (A˚ ).

Mn—O4i

2.148 (3)

Mn—N2 2.257 (3)

Mn—O1W 2.262 (3)

Mn—O2 2.297 (3)

Mn—O1 2.298 (3)

Mn—N1 2.376 (4)

Mn—N3 2.378 (4)

S—O3 1.450 (3)

S—O2 1.457 (3)

S—O4 1.463 (3)

S—O1 1.473 (3)

[image:3.610.312.564.96.142.2]

Symmetry code: (i)x;y;z.

Table 2

Hydrogen-bond geometry (A˚ ,).

D—H A D—H H A D A D—H A

O3W—H3WA O3i

0.83 (4) 2.04 (3) 2.811 (5) 155 (4) O3W—H3WB O3ii

0.83 (4) 2.01 (2) 2.833 (5) 169 (4) O2W—H2WB O4iii

0.83 (4) 2.43 (2) 3.052 (6) 132 (4) O2W—H2WA O3iii

0.83 (4) 2.46 (2) 3.130 (5) 139 (4) O1W—H1WA N6iv 0.83 (4) 2.08 (2) 2.867 (5) 158 (4) O1W—H1WB O3Wv

0.83 (4) 1.98 (2) 2.785 (5) 162 (4)

Symmetry codes: (i) x;y;z; (ii) x;yþ1;z; (iii) xþ1;yþ1;zþ1; (iv)

x;y;zþ1; (v)x;y1;z.

Table 3

–contacts for (I).

Group 1 group 2 cpd (A˚ ) ccd (A˚ ) sa (

)

Cg1 Cg3vi

3.628 (3) 3.36 (2) 22.2 (10) Cg1 Cg4vii

3.593 (3) 3.34 (4) 21.4 (17) Cg2 Cg3iv

3.694 (3) 3.34 (3) 25.4 (9)

cpd: (average) centroid-to-plane distance; ccd: centroid-to-centroid distance; sa: slippage angle (average angle between the intercentroid vector and one plane normal). For symmetry codes, see Table 2.Cg1–Cg4 are the centroids of the rings as defined in Fig. 1.

H atoms attached to C atoms were placed at calculated positions (C—H = 0.93 A˚ ) and refined as riding. H atoms of water molecules were located in difference maps and refined with restrained O—H distances of 0.85 (2) A˚ . The constraintUiso(H) = 1.2Ueq(carrier) was

applied in all cases.

Data collection: SMART-NT (Bruker, 2001); cell refinement:

SAINT-NT(Bruker, 2000); data reduction:SAINT-NT; program(s) used to solve structure: SHELXS97(Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics:XPin SHELXTL/PC(Sheldrick, 1994); software used to prepare material for publication:SHELXL97.

We thank the Spanish Research Council (CSIC) for providing us with a free-of-charge license to the CSD system.

References

Allen, F. H. (2002).Acta Cryst.B58, 380–388.

Bruker (2000). SAINT-NT. Version 6.02a. Bruker AXS Inc., Madison, Wisconsin, USA.

Bruker (2001). SMART-NT. Version 5.624. Bruker AXS Inc., Madison, Wisconsin, USA.

Dı´az de Vivar, E., Baggio, E. & Baggio, R. (2004).Acta Cryst.C60, m495– m497.

Harvey, M., Baggio, S., Pardo, H. & Baggio, R. (2004).Acta Cryst.C60, m79– m81.

Harvey, M., Baggio, S., Russi, S. & Baggio, R. (2003).Acta Cryst.C59, m171– m174.

Remy, H. (1956).Treatise on Inorganic Chemistry.Amsterdam: Elsevier. Sheldrick, G. M. (1994). SHELXTL/PC. Version 5.0. Siemens Analytical

X-ray Instruments Inc., Madison, Wisconsin, USA.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Go¨ttingen, Germany.

Sheldrick, G. M. (2001)SADABS. University of Go¨ttingen, Germany.

metal-organic papers

Acta Cryst.(2006). E62, m141–m143 Dı´az de Vivaret al. [Mn

[image:3.610.43.296.438.510.2]
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supporting information

sup-1

Acta Cryst. (2006). E62, m141–m143

supporting information

Acta Cryst. (2006). E62, m141–m143 [doi:10.1107/S1600536805041528]

Di-

µ

-sulfato-

κ

3

O

,

O

:

O

′′

;

κ

3

O

,

O

:

O

′′

-bis{aqua[2,4,6-tris(2-pyridyl)-1,3,5-triazine-κ

3

N

1

,

N

2

,

N

6

]manganese(II)} tetrahydrate

M. Enriqueta D

í

az de Vivar, Sergio Baggio, Mar

í

a Teresa Garland and Ricardo Baggio

S1. Comment

In the past few years we have reported a number of thiosulfate and sulfite complexes obtained by decomposition of less

common sulfur oxoanions such as dithionite and pyrosulfite. The key argument resides on the instability of these anions

in aqueous solutions (Remy, 1956), which, when interacting with transition metal ions and organic ligands, can produce a

wide variety of transformation products. The high instability, which makes the chemistry of these anions so difficult,

makes them attractive as precursors. Some previously unintentional outcomes (Harvey et al., 2004) suggested, and

further rational synthesis confirmed (Díaz de Vivar et al., 2004), that the method could be an alternative route for the

preparation of thiosulfate or sulfite complexes where direct synthesis had previously proven unsuccessful.

In spite of the achievements of the method in generating interesting structures, the fascinating reactions it promotes

have usualy remained far beyoud the chemist's control and their outcomes have been, more often than not, mainly ruled

by chance. An example of this assertion is presented here, viz. the title compound, [Mn(SO4)(C16H12N6)(H2O)]2·4H2O, (I),

a manganese sulfate complex serendipiously obtained when looking for the thiosulfate analog.

Compound (I) is a dimeric centrosymmetric species isostructural to the Cd analog obtained by a conventional synthesis

starting from a sulfate salt (Harvey et al., 2003). Compound (I) displays a seven-coordinate environment around the Mn

ion, with three N atoms from a tridentate 2,4,6-tris(2-pyridyl)-1,3,5-triazine (tpt) molecule, one O atom from a water

molecule and three further O atoms from two symmetry-related sulfate ions, each one of which binds to two metal

centers, thus generating the dimeric structure (Fig. 1).

The coordination polyhedron about Mn can be described as a distorted pentagonal bipyramid, with the equatorial plane

formed by atoms N1, N2, N3, O1 and O2 [maximum deviation from the mean plane = 0.04 (1) Å for N2] and equatorial

angles subtended at the Mn site ranging from 60.49 (11) to 85.09 (12)° (ideal 72°). The axial sites are occupied by O1w

and O4i [symmetry code: (i) −x, −y, −z] and they subtend an angle of 167.75 (12)° to the cation.

The S—O distances in the sulfate group are all similar (Table 1), suggesting double-bond delocalization. The mean

value [1.461 (9) Å] is similar to that reported for the free anion; a search in the November 2004 version of the Cambridge

Structural Database (Allen, 2002) gave a mean value of 1.472 (8) Å for 118 structures with R < 0.05.

The tpt anion is almost planar and acts as a tridentate species, with its central Mn—N bond [2.257 (3) Å] being

significantly shorter than the lateral ones [2.376 (4) and 2.378 (4) Å]. The ligand does not show any abnormal features,

with its three bound rings being almost coplanar: the atoms deviate on average from an ideal plane by less than 0.02 (1)

Å. The terminal pyridyl moiety deviates from planarity by less than 0.01 (1) Å and subtends to the metal-bonded ring

system by an angle of 3.6 (1)°.

Owing to the dimers building up around an inversion center they present their planar tpt molecules parallel to each

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supporting information

sup-2

Acta Cryst. (2006). E62, m141–m143

sharing one of the two layers in the double molecular units. This disposiiton (Fig. 2) results in a set of interleaved planar

arrays at a nearly graphitic (ca 3.6 Å) distance from one another. Thus, the moleculues of (I) are linked by ππ bonds

between aromatic rings (Table 3) as well as an extensive hydrogen-bonding network having all the available water

molecules as donors and some water O aotms, tpt N atoms and some sulfate O atoms as acceptors (Table 2).

S2. Experimental

A 96% ethanol solution of 2,2′-dipiridilamine was diffused into an equimolar aqueous solution containing MnCl2·4H2O,

sodium dithionite and potassium pyrosulfite (1:1:2 molar ratio). After two weeks a few colorless prisms of (I) suitable for

X-ray analyses were obtained.

S3. Refinement

H atoms attached to C atoms were placed at calculated positions (C—H = 0.93 Å) and refined as riding. H atoms of water

molecules were located in difference maps and refined with restrained O—H distances of 0.85 (2) Å. The constraint

[image:5.610.117.487.278.622.2]

Uiso(H) = 1.2Ueq(host) was applied in all cases.

Figure 1

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supporting information

sup-3

[image:6.610.130.479.68.336.2]

Acta Cryst. (2006). E62, m141–m143 Figure 2

Packing view of (I) along the planes, which are seen as horizontal lines. Selected dimers are drawn in heavy full lines so

as to distinguish them from the background. Hydrogen bonds are shown as dashed lines.

Di-µ-sulfato-κ3O,O′:O′′;κ3O,O′:O′′-bis{aqua[2,4,6-tris(2-pyridyl)- 1,3,5-triazine-κ3N1,N2,N6]manganese(II)}

tetrahydrate

Crystal data

[Mn2(SO4)2(C16H12N6)2(H2O)2]·4H2O

Mr = 1034.77 Triclinic, P1 Hall symbol: -P 1

a = 8.8737 (16) Å

b = 10.5634 (19) Å

c = 12.587 (2) Å

α = 103.566 (3)°

β = 97.981 (3)°

γ = 110.409 (3)°

V = 1042.9 (3) Å3

Z = 1

F(000) = 530

Dx = 1.648 Mg m−3

Mo radiation, λ = 0.71073 Å Cell parameters from 1017 reflections

θ = 5.1–43.9°

µ = 0.79 mm−1

T = 291 K Prism, colorless 0.22 × 0.16 × 0.14 mm

Data collection

Bruker SMART CCD diffractometer

Radiation source: fine-focus sealed tube Graphite monochromator

φ and ω scans

Absorption correction: multi-scan (SADABS; Sheldrick, 2001)

Tmin = 0.846, Tmax = 0.898

8696 measured reflections 4041 independent reflections 2775 reflections with I > 2σ(I)

Rint = 0.058

θmax = 26.0°, θmin = 1.7°

h = −10→10

k = −13→12

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Acta Cryst. (2006). E62, m141–m143 Refinement

Refinement on F2

Least-squares matrix: full

R[F2 > 2σ(F2)] = 0.066

wR(F2) = 0.109

S = 1.05 4041 reflections 319 parameters 13 restraints

Primary atom site location: structure-invariant direct methods

Secondary atom site location: difference Fourier map

Hydrogen site location: inferred from neighbouring sites

H atoms treated by a mixture of independent and constrained refinement

w = 1/[σ2(F

o2) + (0.013P)2 + 2.08P]

where P = (Fo2 + 2Fc2)/3

(Δ/σ)max = 0.026

Δρmax = 0.46 e Å−3

Δρmin = −0.39 e Å−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

x y z Uiso*/Ueq

Mn 0.08793 (9) −0.00477 (7) 0.18395 (6) 0.0322 (2) S −0.00324 (15) −0.20172 (12) −0.03890 (10) 0.0339 (3)

O1 0.1636 (4) −0.0991 (4) 0.0266 (3) 0.0535 (9)

O2 −0.1108 (4) −0.1846 (3) 0.0360 (3) 0.0476 (8)

O3 −0.0078 (5) −0.3444 (3) −0.0699 (3) 0.0562 (9) O4 −0.0533 (4) −0.1707 (3) −0.1423 (3) 0.0479 (8)

N1 0.3790 (5) 0.1289 (4) 0.2420 (3) 0.0366 (10)

N2 0.1627 (4) 0.1351 (4) 0.3642 (3) 0.0296 (9)

N3 −0.1453 (5) −0.0318 (4) 0.2632 (3) 0.0324 (9)

N4 0.3713 (5) 0.3076 (4) 0.5194 (3) 0.0379 (10)

N5 0.0920 (5) 0.2204 (4) 0.5326 (3) 0.0336 (9)

N6 0.1878 (5) 0.3821 (4) 0.7507 (3) 0.0408 (10)

C1 0.4866 (7) 0.1244 (5) 0.1782 (5) 0.0491 (14)

H1A 0.4457 0.0650 0.1043 0.059*

C2 0.6538 (7) 0.2024 (6) 0.2159 (5) 0.0532 (15)

H2A 0.7237 0.1951 0.1682 0.064*

C3 0.7176 (6) 0.2916 (6) 0.3245 (5) 0.0517 (14)

H3A 0.8309 0.3448 0.3518 0.062*

C4 0.6106 (6) 0.3005 (5) 0.3918 (5) 0.0473 (14)

H4A 0.6495 0.3602 0.4657 0.057*

C5 0.4436 (6) 0.2185 (5) 0.3474 (4) 0.0321 (11)

C6 0.3202 (5) 0.2225 (5) 0.4149 (4) 0.0303 (11)

C7 0.2523 (6) 0.3022 (5) 0.5748 (4) 0.0352 (11)

C8 0.0548 (5) 0.1394 (4) 0.4272 (4) 0.0290 (10)

C9 −0.1206 (5) 0.0439 (4) 0.3712 (4) 0.0284 (10)

C10 −0.2459 (6) 0.0329 (5) 0.4254 (4) 0.0391 (12)

H10A −0.2234 0.0862 0.5002 0.047*

C11 −0.4039 (6) −0.0570 (5) 0.3684 (4) 0.0436 (13)

H11A −0.4906 −0.0664 0.4038 0.052*

C12 −0.4331 (6) −0.1339 (5) 0.2575 (4) 0.0434 (13)

H12A −0.5399 −0.1953 0.2162 0.052*

C13 −0.2998 (6) −0.1174 (5) 0.2089 (4) 0.0403 (12)

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Acta Cryst. (2006). E62, m141–m143

C14 0.3072 (6) 0.3939 (5) 0.6944 (4) 0.0334 (11)

C15 0.4708 (6) 0.4828 (5) 0.7432 (4) 0.0444 (13)

H15A 0.5505 0.4872 0.7018 0.053*

C16 0.5140 (6) 0.5636 (5) 0.8519 (4) 0.0469 (14)

H16A 0.6237 0.6248 0.8861 0.056*

C17 0.3942 (6) 0.5542 (5) 0.9109 (4) 0.0477 (14)

H17A 0.4207 0.6088 0.9858 0.057*

C18 0.2355 (7) 0.4629 (5) 0.8576 (4) 0.0485 (14)

H18A 0.1551 0.4567 0.8985 0.058*

O1W 0.1254 (4) −0.1645 (3) 0.2654 (3) 0.0420 (9)

H1WA 0.038 (4) −0.214 (3) 0.279 (4) 0.050*

H1WB 0.167 (5) −0.214 (3) 0.228 (4) 0.050*

O2W 0.8636 (6) 0.5572 (6) 0.6678 (4) 0.118 (2)

H2WA 0.894 (4) 0.539 (3) 0.7259 (18) 0.141*

H2WB 0.867 (4) 0.639 (2) 0.6819 (19) 0.141*

O3W 0.1945 (4) 0.6358 (3) 0.1152 (3) 0.0495 (10)

H3WA 0.169 (6) 0.550 (2) 0.106 (3) 0.059*

H3WB 0.146 (6) 0.651 (4) 0.061 (3) 0.059*

Atomic displacement parameters (Å2)

U11 U22 U33 U12 U13 U23

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Acta Cryst. (2006). E62, m141–m143

C15 0.037 (3) 0.042 (3) 0.051 (3) 0.012 (3) 0.010 (3) 0.015 (3) C16 0.042 (3) 0.038 (3) 0.039 (3) 0.002 (3) −0.003 (3) −0.001 (2) C17 0.051 (4) 0.039 (3) 0.038 (3) 0.008 (3) 0.006 (3) 0.004 (3) C18 0.059 (4) 0.043 (3) 0.039 (3) 0.014 (3) 0.024 (3) 0.006 (3) O1W 0.045 (2) 0.041 (2) 0.046 (2) 0.0166 (17) 0.0223 (17) 0.0154 (17) O2W 0.085 (4) 0.158 (5) 0.052 (3) −0.001 (4) 0.011 (3) 0.008 (3) O3W 0.052 (2) 0.039 (2) 0.052 (2) 0.0203 (19) 0.0018 (19) 0.0078 (18)

Geometric parameters (Å, º)

Mn—O4i 2.148 (3) C3—H3A 0.9300

Mn—N2 2.257 (3) C4—C5 1.381 (6)

Mn—O1W 2.262 (3) C4—H4A 0.9300

Mn—O2 2.297 (3) C5—C6 1.481 (6)

Mn—O1 2.298 (3) C7—C14 1.491 (6)

Mn—N1 2.376 (4) C8—C9 1.485 (6)

Mn—N3 2.378 (4) C9—C10 1.368 (6)

S—O3 1.450 (3) C10—C11 1.362 (6)

S—O2 1.457 (3) C10—H10A 0.9300

S—O4 1.463 (3) C11—C12 1.377 (6)

S—O1 1.473 (3) C11—H11A 0.9300

O4—Mni 2.148 (3) C12—C13 1.382 (6)

N1—C1 1.336 (6) C12—H12A 0.9300

N1—C5 1.343 (6) C13—H13A 0.9300

N2—C8 1.331 (5) C14—C15 1.377 (6)

N2—C6 1.338 (5) C15—C16 1.351 (6)

N3—C13 1.323 (5) C15—H15A 0.9300

N3—C9 1.350 (5) C16—C17 1.369 (7)

N4—C6 1.320 (5) C16—H16A 0.9300

N4—C7 1.336 (5) C17—C18 1.360 (7)

N5—C8 1.323 (5) C17—H17A 0.9300

N5—C7 1.330 (5) C18—H18A 0.9300

N6—C18 1.330 (6) O1W—H1WA 0.83 (4)

N6—C14 1.341 (5) O1W—H1WB 0.83 (4)

C1—C2 1.369 (7) O2W—H2WA 0.83 (4)

C1—H1A 0.9300 O2W—H2WB 0.83 (4)

C2—C3 1.373 (7) O3W—H3WA 0.83 (4)

C2—H2A 0.9300 O3W—H3WB 0.83 (4)

C3—C4 1.370 (7)

O4i—Mn—O1W 167.75 (12) C4—C3—H3A 120.7

O4i—Mn—N1 90.03 (13) C2—C3—H3A 120.7

O4i—Mn—N2 85.09 (12) C3—C4—C5 118.4 (5)

O4i—Mn—N3 86.45 (13) C3—C4—H4A 120.8

O4i—Mn—O1 99.97 (13) C5—C4—H4A 120.8

O4i—Mn—O2 98.15 (13) N1—C5—C4 124.0 (4)

O1W—Mn—N1 88.63 (12) N1—C5—C6 114.5 (4)

(10)

supporting information

sup-7

Acta Cryst. (2006). E62, m141–m143

O1W—Mn—N3 86.35 (12) N4—C6—N2 124.7 (4)

O1W—Mn—O1 91.80 (13) N4—C6—C5 119.1 (4)

O1W—Mn—O2 90.55 (12) N2—C6—C5 116.2 (4)

O2—Mn—O1 60.49 (11) N5—C7—N4 125.4 (4)

O1—Mn—N1 80.35 (12) N5—C7—C14 118.4 (4)

N1—Mn—N2 69.08 (13) N4—C7—C14 116.2 (4)

N2—Mn—N3 68.52 (13) N5—C8—N2 125.5 (4)

N3—Mn—O2 81.38 (12) N5—C8—C9 119.2 (4)

N2—Mn—O2 149.52 (12) N2—C8—C9 115.3 (4)

N2—Mn—O1 149.06 (13) N3—C9—C10 123.0 (4)

O2—Mn—N1 140.79 (12) N3—C9—C8 114.4 (4)

O1—Mn—N3 141.83 (12) C10—C9—C8 122.6 (4)

N1—Mn—N3 137.59 (13) C11—C10—C9 119.2 (4)

O3—S—O2 112.2 (2) C11—C10—H10A 120.4

O3—S—O4 108.09 (19) C9—C10—H10A 120.4

O2—S—O4 110.3 (2) C10—C11—C12 119.0 (4)

O3—S—O1 110.4 (2) C10—C11—H11A 120.5

O2—S—O1 104.37 (19) C12—C11—H11A 120.5

O4—S—O1 111.5 (2) C11—C12—C13 118.3 (5)

O3—S—Mn 127.87 (15) C11—C12—H12A 120.8

O2—S—Mn 52.15 (13) C13—C12—H12A 120.8

O4—S—Mn 124.04 (14) N3—C13—C12 123.6 (4)

O1—S—Mn 52.25 (13) N3—C13—H13A 118.2

S—O1—Mn 97.30 (16) C12—C13—H13A 118.2

S—O2—Mn 97.79 (17) N6—C14—C15 122.8 (5)

S—O4—Mni 136.16 (19) N6—C14—C7 115.6 (4)

C1—N1—C5 116.0 (4) C15—C14—C7 121.6 (4)

C1—N1—Mn 125.6 (3) C16—C15—C14 119.2 (5)

C5—N1—Mn 118.4 (3) C16—C15—H15A 120.4

C8—N2—C6 115.0 (4) C14—C15—H15A 120.4

C8—N2—Mn 123.2 (3) C15—C16—C17 119.1 (5)

C6—N2—Mn 121.8 (3) C15—C16—H16A 120.4

C13—N3—C9 116.8 (4) C17—C16—H16A 120.4

C13—N3—Mn 124.6 (3) C18—C17—C16 118.4 (5)

C9—N3—Mn 118.6 (3) C18—C17—H17A 120.8

C6—N4—C7 115.1 (4) C16—C17—H17A 120.8

C8—N5—C7 114.4 (4) N6—C18—C17 124.3 (5)

C18—N6—C14 116.1 (4) N6—C18—H18A 117.8

N1—C1—C2 123.5 (5) C17—C18—H18A 117.8

N1—C1—H1A 118.2 Mn—O1W—H1WA 112 (3)

C2—C1—H1A 118.2 Mn—O1W—H1WB 112 (3)

C1—C2—C3 119.5 (5) H1WA—O1W—H1WB 112 (4)

C1—C2—H2A 120.2 H2WA—O2W—H2WB 112 (5)

C3—C2—H2A 120.3 H3WA—O3W—H3WB 112 (4)

C4—C3—C2 118.6 (5)

(11)

supporting information

sup-8

Acta Cryst. (2006). E62, m141–m143 Hydrogen-bond geometry (Å, º)

D—H···A D—H H···A D···A D—H···A

O3W—H3WA···O3i 0.83 (4) 2.04 (3) 2.811 (5) 155 (4)

O3W—H3WB···O3ii 0.83 (4) 2.01 (2) 2.833 (5) 169 (4)

O2W—H2WB···O4iii 0.83 (4) 2.43 (2) 3.052 (6) 132 (4)

O2W—H2WA···O3iii 0.83 (4) 2.46 (2) 3.130 (5) 139 (4)

O1W—H1WA···N6iv 0.83 (4) 2.08 (2) 2.867 (5) 158 (4)

O1W—H1WB···O3Wv 0.83 (4) 1.98 (2) 2.785 (5) 162 (4)

Figure

Figure 2Packing view of (I) along the planes, which are seen as horizontal lines.Selected dimers are drawn in heavy full lines so as to distinguish themfrom the background
Table 3
Figure 1
Figure 2

References

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