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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805041528/hb6305sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805041528/hb6305Isup2.hkl
Contains datablock I

CCDC reference: 296565

Key indicators

  • Single-crystal X-ray study
  • T = 291 K
  • Mean [sigma](C-C) = 0.008 Å
  • R factor = 0.066
  • wR factor = 0.109
  • Data-to-parameter ratio = 12.7

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn - O1 .. 5.13 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn - O1W .. 6.49 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Comment top

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 other. Crystal symmetry preserves the orientation of the dimeric units, which stack in sets of parallel planes, alternatively 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).

Experimental top

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.

Refinement top

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

Computing details top

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: XP in SHELXTL/PC (Sheldrick, 1994); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. : View of (I), showing 50% displacement ellipsoids. [Symmetry code: (i) −x, −y, −z.
[Figure 2] Fig. 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 top
Crystal data top
[Mn2(SO4)2(C16H12N6)2(H2O)2]·4H2OZ = 1
Mr = 1034.77F(000) = 530
Triclinic, P1Dx = 1.648 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.8737 (16) ÅCell parameters from 1017 reflections
b = 10.5634 (19) Åθ = 5.1–43.9°
c = 12.587 (2) ŵ = 0.79 mm1
α = 103.566 (3)°T = 291 K
β = 97.981 (3)°Prism, colorless
γ = 110.409 (3)°0.22 × 0.16 × 0.14 mm
V = 1042.9 (3) Å3
Data collection top
Bruker SMART CCD
diffractometer
4041 independent reflections
Radiation source: fine-focus sealed tube2775 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.058
ϕ and ω scansθmax = 26.0°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
h = 1010
Tmin = 0.846, Tmax = 0.898k = 1312
8696 measured reflectionsl = 1615
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)] = 0.066Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.109H atoms treated by a mixture of independent and constrained refinement
S = 1.05 w = 1/[σ2(Fo2) + (0.013P)2 + 2.08P]
where P = (Fo2 + 2Fc2)/3
4041 reflections(Δ/σ)max = 0.026
319 parametersΔρmax = 0.46 e Å3
13 restraintsΔρmin = 0.39 e Å3
Crystal data top
[Mn2(SO4)2(C16H12N6)2(H2O)2]·4H2Oγ = 110.409 (3)°
Mr = 1034.77V = 1042.9 (3) Å3
Triclinic, P1Z = 1
a = 8.8737 (16) ÅMo Kα radiation
b = 10.5634 (19) ŵ = 0.79 mm1
c = 12.587 (2) ÅT = 291 K
α = 103.566 (3)°0.22 × 0.16 × 0.14 mm
β = 97.981 (3)°
Data collection top
Bruker SMART CCD
diffractometer
4041 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 2001)
2775 reflections with I > 2σ(I)
Tmin = 0.846, Tmax = 0.898Rint = 0.058
8696 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.06613 restraints
wR(F2) = 0.109H atoms treated by a mixture of independent and constrained refinement
S = 1.05Δρmax = 0.46 e Å3
4041 reflectionsΔρmin = 0.39 e Å3
319 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mn0.08793 (9)0.00477 (7)0.18395 (6)0.0322 (2)
S0.00324 (15)0.20172 (12)0.03890 (10)0.0339 (3)
O10.1636 (4)0.0991 (4)0.0266 (3)0.0535 (9)
O20.1108 (4)0.1846 (3)0.0360 (3)0.0476 (8)
O30.0078 (5)0.3444 (3)0.0699 (3)0.0562 (9)
O40.0533 (4)0.1707 (3)0.1423 (3)0.0479 (8)
N10.3790 (5)0.1289 (4)0.2420 (3)0.0366 (10)
N20.1627 (4)0.1351 (4)0.3642 (3)0.0296 (9)
N30.1453 (5)0.0318 (4)0.2632 (3)0.0324 (9)
N40.3713 (5)0.3076 (4)0.5194 (3)0.0379 (10)
N50.0920 (5)0.2204 (4)0.5326 (3)0.0336 (9)
N60.1878 (5)0.3821 (4)0.7507 (3)0.0408 (10)
C10.4866 (7)0.1244 (5)0.1782 (5)0.0491 (14)
H1A0.44570.06500.10430.059*
C20.6538 (7)0.2024 (6)0.2159 (5)0.0532 (15)
H2A0.72370.19510.16820.064*
C30.7176 (6)0.2916 (6)0.3245 (5)0.0517 (14)
H3A0.83090.34480.35180.062*
C40.6106 (6)0.3005 (5)0.3918 (5)0.0473 (14)
H4A0.64950.36020.46570.057*
C50.4436 (6)0.2185 (5)0.3474 (4)0.0321 (11)
C60.3202 (5)0.2225 (5)0.4149 (4)0.0303 (11)
C70.2523 (6)0.3022 (5)0.5748 (4)0.0352 (11)
C80.0548 (5)0.1394 (4)0.4272 (4)0.0290 (10)
C90.1206 (5)0.0439 (4)0.3712 (4)0.0284 (10)
C100.2459 (6)0.0329 (5)0.4254 (4)0.0391 (12)
H10A0.22340.08620.50020.047*
C110.4039 (6)0.0570 (5)0.3684 (4)0.0436 (13)
H11A0.49060.06640.40380.052*
C120.4331 (6)0.1339 (5)0.2575 (4)0.0434 (13)
H12A0.53990.19530.21620.052*
C130.2998 (6)0.1174 (5)0.2089 (4)0.0403 (12)
H13A0.31990.16950.13400.048*
C140.3072 (6)0.3939 (5)0.6944 (4)0.0334 (11)
C150.4708 (6)0.4828 (5)0.7432 (4)0.0444 (13)
H15A0.55050.48720.70180.053*
C160.5140 (6)0.5636 (5)0.8519 (4)0.0469 (14)
H16A0.62370.62480.88610.056*
C170.3942 (6)0.5542 (5)0.9109 (4)0.0477 (14)
H17A0.42070.60880.98580.057*
C180.2355 (7)0.4629 (5)0.8576 (4)0.0485 (14)
H18A0.15510.45670.89850.058*
O1W0.1254 (4)0.1645 (3)0.2654 (3)0.0420 (9)
H1WA0.038 (4)0.214 (3)0.279 (4)0.050*
H1WB0.167 (5)0.214 (3)0.228 (4)0.050*
O2W0.8636 (6)0.5572 (6)0.6678 (4)0.118 (2)
H2WA0.894 (4)0.539 (3)0.7259 (18)0.141*
H2WB0.867 (4)0.639 (2)0.6819 (19)0.141*
O3W0.1945 (4)0.6358 (3)0.1152 (3)0.0495 (10)
H3WA0.169 (6)0.550 (2)0.106 (3)0.059*
H3WB0.146 (6)0.651 (4)0.061 (3)0.059*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn0.0397 (5)0.0299 (4)0.0298 (4)0.0133 (3)0.0158 (3)0.0104 (3)
S0.0452 (7)0.0296 (6)0.0301 (6)0.0160 (6)0.0142 (5)0.0097 (5)
O10.0465 (14)0.0568 (19)0.0414 (17)0.0125 (14)0.0139 (12)0.0028 (15)
O20.0507 (16)0.049 (2)0.0371 (16)0.0159 (14)0.0191 (12)0.0038 (12)
O30.092 (3)0.0351 (14)0.049 (2)0.0347 (17)0.0171 (19)0.0102 (13)
O40.078 (2)0.0403 (19)0.0322 (12)0.0298 (18)0.0150 (14)0.0120 (13)
N10.042 (2)0.035 (2)0.043 (2)0.017 (2)0.024 (2)0.019 (2)
N20.033 (2)0.030 (2)0.029 (2)0.0144 (18)0.0133 (18)0.0084 (17)
N30.034 (2)0.028 (2)0.032 (2)0.0109 (18)0.0108 (18)0.0062 (18)
N40.036 (2)0.039 (2)0.038 (2)0.012 (2)0.015 (2)0.013 (2)
N50.036 (2)0.034 (2)0.027 (2)0.0108 (19)0.0111 (18)0.0067 (18)
N60.040 (3)0.036 (2)0.040 (3)0.007 (2)0.017 (2)0.011 (2)
C10.056 (4)0.049 (3)0.055 (3)0.026 (3)0.030 (3)0.020 (3)
C20.053 (4)0.060 (4)0.070 (4)0.028 (3)0.043 (3)0.035 (3)
C30.034 (3)0.048 (3)0.072 (4)0.011 (3)0.015 (3)0.024 (3)
C40.037 (3)0.052 (3)0.059 (4)0.016 (3)0.021 (3)0.026 (3)
C50.038 (3)0.028 (3)0.039 (3)0.017 (2)0.018 (2)0.015 (2)
C60.029 (3)0.028 (3)0.037 (3)0.010 (2)0.012 (2)0.015 (2)
C70.035 (3)0.031 (3)0.043 (3)0.011 (2)0.013 (2)0.018 (2)
C80.036 (3)0.029 (3)0.032 (3)0.016 (2)0.016 (2)0.018 (2)
C90.028 (3)0.026 (2)0.030 (3)0.009 (2)0.009 (2)0.009 (2)
C100.038 (3)0.041 (3)0.037 (3)0.011 (2)0.016 (2)0.013 (2)
C110.038 (3)0.042 (3)0.054 (3)0.015 (3)0.025 (3)0.015 (3)
C120.025 (3)0.037 (3)0.053 (3)0.002 (2)0.005 (2)0.006 (3)
C130.039 (3)0.043 (3)0.035 (3)0.014 (3)0.009 (2)0.006 (2)
C140.038 (3)0.028 (3)0.036 (3)0.012 (2)0.010 (2)0.012 (2)
C150.037 (3)0.042 (3)0.051 (3)0.012 (3)0.010 (3)0.015 (3)
C160.042 (3)0.038 (3)0.039 (3)0.002 (3)0.003 (3)0.001 (2)
C170.051 (4)0.039 (3)0.038 (3)0.008 (3)0.006 (3)0.004 (3)
C180.059 (4)0.043 (3)0.039 (3)0.014 (3)0.024 (3)0.006 (3)
O1W0.045 (2)0.041 (2)0.046 (2)0.0166 (17)0.0223 (17)0.0154 (17)
O2W0.085 (4)0.158 (5)0.052 (3)0.001 (4)0.011 (3)0.008 (3)
O3W0.052 (2)0.039 (2)0.052 (2)0.0203 (19)0.0018 (19)0.0078 (18)
Geometric parameters (Å, º) top
Mn—O4i2.148 (3)C3—H3A0.9300
Mn—N22.257 (3)C4—C51.381 (6)
Mn—O1W2.262 (3)C4—H4A0.9300
Mn—O22.297 (3)C5—C61.481 (6)
Mn—O12.298 (3)C7—C141.491 (6)
Mn—N12.376 (4)C8—C91.485 (6)
Mn—N32.378 (4)C9—C101.368 (6)
S—O31.450 (3)C10—C111.362 (6)
S—O21.457 (3)C10—H10A0.9300
S—O41.463 (3)C11—C121.377 (6)
S—O11.473 (3)C11—H11A0.9300
O4—Mni2.148 (3)C12—C131.382 (6)
N1—C11.336 (6)C12—H12A0.9300
N1—C51.343 (6)C13—H13A0.9300
N2—C81.331 (5)C14—C151.377 (6)
N2—C61.338 (5)C15—C161.351 (6)
N3—C131.323 (5)C15—H15A0.9300
N3—C91.350 (5)C16—C171.369 (7)
N4—C61.320 (5)C16—H16A0.9300
N4—C71.336 (5)C17—C181.360 (7)
N5—C81.323 (5)C17—H17A0.9300
N5—C71.330 (5)C18—H18A0.9300
N6—C181.330 (6)O1W—H1WA0.83 (4)
N6—C141.341 (5)O1W—H1WB0.83 (4)
C1—C21.369 (7)O2W—H2WA0.83 (4)
C1—H1A0.9300O2W—H2WB0.83 (4)
C2—C31.373 (7)O3W—H3WA0.83 (4)
C2—H2A0.9300O3W—H3WB0.83 (4)
C3—C41.370 (7)
O4i—Mn—O1W167.75 (12)C4—C3—H3A120.7
O4i—Mn—N190.03 (13)C2—C3—H3A120.7
O4i—Mn—N285.09 (12)C3—C4—C5118.4 (5)
O4i—Mn—N386.45 (13)C3—C4—H4A120.8
O4i—Mn—O199.97 (13)C5—C4—H4A120.8
O4i—Mn—O298.15 (13)N1—C5—C4124.0 (4)
O1W—Mn—N188.63 (12)N1—C5—C6114.5 (4)
O1W—Mn—N283.06 (12)C4—C5—C6121.5 (4)
O1W—Mn—N386.35 (12)N4—C6—N2124.7 (4)
O1W—Mn—O191.80 (13)N4—C6—C5119.1 (4)
O1W—Mn—O290.55 (12)N2—C6—C5116.2 (4)
O2—Mn—O160.49 (11)N5—C7—N4125.4 (4)
O1—Mn—N180.35 (12)N5—C7—C14118.4 (4)
N1—Mn—N269.08 (13)N4—C7—C14116.2 (4)
N2—Mn—N368.52 (13)N5—C8—N2125.5 (4)
N3—Mn—O281.38 (12)N5—C8—C9119.2 (4)
N2—Mn—O2149.52 (12)N2—C8—C9115.3 (4)
N2—Mn—O1149.06 (13)N3—C9—C10123.0 (4)
O2—Mn—N1140.79 (12)N3—C9—C8114.4 (4)
O1—Mn—N3141.83 (12)C10—C9—C8122.6 (4)
N1—Mn—N3137.59 (13)C11—C10—C9119.2 (4)
O3—S—O2112.2 (2)C11—C10—H10A120.4
O3—S—O4108.09 (19)C9—C10—H10A120.4
O2—S—O4110.3 (2)C10—C11—C12119.0 (4)
O3—S—O1110.4 (2)C10—C11—H11A120.5
O2—S—O1104.37 (19)C12—C11—H11A120.5
O4—S—O1111.5 (2)C11—C12—C13118.3 (5)
O3—S—Mn127.87 (15)C11—C12—H12A120.8
O2—S—Mn52.15 (13)C13—C12—H12A120.8
O4—S—Mn124.04 (14)N3—C13—C12123.6 (4)
O1—S—Mn52.25 (13)N3—C13—H13A118.2
S—O1—Mn97.30 (16)C12—C13—H13A118.2
S—O2—Mn97.79 (17)N6—C14—C15122.8 (5)
S—O4—Mni136.16 (19)N6—C14—C7115.6 (4)
C1—N1—C5116.0 (4)C15—C14—C7121.6 (4)
C1—N1—Mn125.6 (3)C16—C15—C14119.2 (5)
C5—N1—Mn118.4 (3)C16—C15—H15A120.4
C8—N2—C6115.0 (4)C14—C15—H15A120.4
C8—N2—Mn123.2 (3)C15—C16—C17119.1 (5)
C6—N2—Mn121.8 (3)C15—C16—H16A120.4
C13—N3—C9116.8 (4)C17—C16—H16A120.4
C13—N3—Mn124.6 (3)C18—C17—C16118.4 (5)
C9—N3—Mn118.6 (3)C18—C17—H17A120.8
C6—N4—C7115.1 (4)C16—C17—H17A120.8
C8—N5—C7114.4 (4)N6—C18—C17124.3 (5)
C18—N6—C14116.1 (4)N6—C18—H18A117.8
N1—C1—C2123.5 (5)C17—C18—H18A117.8
N1—C1—H1A118.2Mn—O1W—H1WA112 (3)
C2—C1—H1A118.2Mn—O1W—H1WB112 (3)
C1—C2—C3119.5 (5)H1WA—O1W—H1WB112 (4)
C1—C2—H2A120.2H2WA—O2W—H2WB112 (5)
C3—C2—H2A120.3H3WA—O3W—H3WB112 (4)
C4—C3—C2118.6 (5)
Symmetry code: (i) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3W—H3WA···O3i0.83 (4)2.04 (3)2.811 (5)155 (4)
O3W—H3WB···O3ii0.83 (4)2.01 (2)2.833 (5)169 (4)
O2W—H2WB···O4iii0.83 (4)2.43 (2)3.052 (6)132 (4)
O2W—H2WA···O3iii0.83 (4)2.46 (2)3.130 (5)139 (4)
O1W—H1WA···N6iv0.83 (4)2.08 (2)2.867 (5)158 (4)
O1W—H1WB···O3Wv0.83 (4)1.98 (2)2.785 (5)162 (4)
Symmetry codes: (i) x, y, z; (ii) x, y+1, z; (iii) x+1, y+1, z+1; (iv) x, y, z+1; (v) x, y1, z.

Experimental details

Crystal data
Chemical formula[Mn2(SO4)2(C16H12N6)2(H2O)2]·4H2O
Mr1034.77
Crystal system, space groupTriclinic, P1
Temperature (K)291
a, b, c (Å)8.8737 (16), 10.5634 (19), 12.587 (2)
α, β, γ (°)103.566 (3), 97.981 (3), 110.409 (3)
V3)1042.9 (3)
Z1
Radiation typeMo Kα
µ (mm1)0.79
Crystal size (mm)0.22 × 0.16 × 0.14
Data collection
DiffractometerBruker SMART CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2001)
Tmin, Tmax0.846, 0.898
No. of measured, independent and
observed [I > 2σ(I)] reflections
8696, 4041, 2775
Rint0.058
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.066, 0.109, 1.05
No. of reflections4041
No. of parameters319
No. of restraints13
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.46, 0.39

Computer programs: SMART-NT (Bruker, 2001), SAINT-NT (Bruker, 2000), SAINT-NT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP in SHELXTL/PC (Sheldrick, 1994), SHELXL97.

Selected bond lengths (Å) top
Mn—O4i2.148 (3)Mn—N32.378 (4)
Mn—N22.257 (3)S—O31.450 (3)
Mn—O1W2.262 (3)S—O21.457 (3)
Mn—O22.297 (3)S—O41.463 (3)
Mn—O12.298 (3)S—O11.473 (3)
Mn—N12.376 (4)
Symmetry code: (i) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3W—H3WA···O3i0.83 (4)2.04 (3)2.811 (5)155 (4)
O3W—H3WB···O3ii0.83 (4)2.01 (2)2.833 (5)169 (4)
O2W—H2WB···O4iii0.83 (4)2.43 (2)3.052 (6)132 (4)
O2W—H2WA···O3iii0.83 (4)2.46 (2)3.130 (5)139 (4)
O1W—H1WA···N6iv0.83 (4)2.08 (2)2.867 (5)158 (4)
O1W—H1WB···O3Wv0.83 (4)1.98 (2)2.785 (5)162 (4)
Symmetry codes: (i) x, y, z; (ii) x, y+1, z; (iii) x+1, y+1, z+1; (iv) x, y, z+1; (v) x, y1, z.
ππ contacts for (I) top
Group 1···Group 2cpd(Å)ccd(Å)sa(°)
Cg1···Cg3vi3.628 (3)3.36 (2)22.2 (10)
Cg1···Cg4vii3.593 (3)3.34 (4)21.4 (17)
Cg2···Cg3iv3.694 (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 the, non strictly parallel, plane normals. For symmetry codes, see Table 2. Cg1–Cg4 are defined in Fig. 1.
 

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