metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 70| Part 5| May 2014| Pages m170-m171

Poly[[tetra-μ-cyanido-κ8C:N-dodeca-cyanido-κ12C-tris­­(N,N-di­methyl­formamide-κO)tris­­(methanol-κO)tris­­(3,4,7,8-tetra­methyl-1,10-phenanthroline-κ2N,N′)trimanganese(II)ditungstate(V)] dihydrate]

aSchool of Environmental and Chemical Engineering, Jiangsu University of Science and Technology, Zhenjiang 212003, People's Republic of China
*Correspondence e-mail: aihua.yuan@just.edu.cn

(Received 26 March 2014; accepted 1 April 2014; online 5 April 2014)

The asymmetric unit of the title compound, {[Mn3{W(CN)8}2(C16H16N2)3(C3H7NO)3(CH3OH)3]·2H2O}n, consists of three [Mn(N,N-di­methyl­formamide)(methanol)(3,4,7,8-tetra­methyl-1,10-phenanthroline)]2+ cations, two [W(CN)8]3− anions and two water mol­ecules. Each water mol­ecule is disordered over three sets of sites, with a refined occupancy ratio of 0.310 (9):0.275 (9):0.415 (9) for one mol­ecule and 0.335 (9):0.288 (9):0.377 (9) for the other mol­ecule. The MnII atoms exhibit a distorted octa­hedral geometry, while the WV atoms adopt a distorted square-anti­prismatic geometry. The MnII and WV atoms are linked alternatively through cyanide groups, forming a tetra­nuclear 12-atom rhombic metallacycle. Adjacent metallacycles are further connected by μ2-bridging cyanide anions, generating a 3,2-chain structure running parallel to [101]. Inter­chain ππ inter­actions are observed [centroid–centroid distances = 3.763 (3) and 3.620 (2) Å].

Related literature

For general background to octacyanidometalate-based compounds, see: Nowicka et al. (2012[Nowicka, B., Korzeniak, T., Stefańczyk, O., Pinkowicz, D., Chorąży, S., Podgajny, R. & Sieklucka, B. (2012). Coord. Chem. Rev. 256, 1946-1971.]); Sieklucka et al. (2011[Sieklucka, B., Podgajny, R., Korzeniak, T., Nowicka, B., Pinkowicz, D. & Kozieł, M. (2011). Eur. J. Inorg. Chem. pp. 305-326.]). For related structures, see: Li et al. (2002[Li, D. F., Gao, S., Zheng, L. M. & Tang, W. X. (2002). J. Chem. Soc. Dalton Trans. pp. 2805-2806.], 2003[Li, D. F., Zheng, L. M., Zhang, Y. Z., Huang, J., Gao, S. & Tang, W. X. (2003). Inorg. Chem. 42, 6123-6129.]); Withers et al. (2007[Withers, J. R., Li, D. F., Triplet, J., Ruschman, C., Parkin, S., Wang, G. B., Yee, G. T. & Holmes, S. M. (2007). Polyhedron, 26, 2353-2366.]). For the synthesis of octacyanidotungstate(V), see: Bok et al. (1975[Bok, L. D. C., Leipoldt, J. G. & Basson, S. S. (1975). Z. Anorg. Allg. Chem. 415, 81-83.]).

[Scheme 1]

Experimental

Crystal data
  • [Mn3W2(CN)16(C16H16N2)3(C3H7NO)3(CH4O)3]·2H2O

  • Mr = 2009.20

  • Triclinic, [P \overline 1]

  • a = 15.5038 (17) Å

  • b = 16.4958 (18) Å

  • c = 21.4067 (13) Å

  • α = 70.008 (2)°

  • β = 82.663 (3)°

  • γ = 66.129 (2)°

  • V = 4704.4 (8) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 2.89 mm−1

  • T = 291 K

  • 0.24 × 0.20 × 0.18 mm

Data collection
  • Bruker SMART APEXII diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2004[Bruker (2004). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.50, Tmax = 0.60

  • 35664 measured reflections

  • 17934 independent reflections

  • 14773 reflections with I > 2σ(I)

  • Rint = 0.016

Refinement
  • R[F2 > 2σ(F2)] = 0.046

  • wR(F2) = 0.117

  • S = 1.05

  • 17934 reflections

  • 1078 parameters

  • 2 restraints

  • H-atom parameters constrained

  • Δρmax = 1.38 e Å−3

  • Δρmin = −0.92 e Å−3

Data collection: APEX2 (Bruker, 2004[Bruker (2004). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2004[Bruker (2004). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2006[Brandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]).

Supporting information


Comment top

Recently, increasing attention has been put into the design and syntheses of functional materials, among which octacyanometalates [M(CN)8]n- (M = Mo, W; n = 3, 4) with flexible coordination modes and low symmetries have been widely studied (Nowicka et al., 2012; Sieklucka et al., 2011). For such systems, chelated ligands are usually employed to control on metal centers for CN-bridging, hence generating low-dimensional architectures rather than extended networks. As a part of a detailed study of cyano-bridged assemblies, we used [W(CN)8]3- as precursor to react with Mn2+ ions and the chelated ligand 3,4,7,8-tetramethyl-1,10-phenanthroline (tmphen), and a new bimetallic compound with 3,2 chain structure was obtained.

The asymmetric unit of the title compound (Fig. 1) consists of three [Mn(3,4,7,8-tetramethyl-1,10-phenanthroline)(methanol)(N,N-dimethylformamide)]2+ cations, two [W(CN)8]3- anions, and two disordered water molecules of crystallization. The Mn atoms exhibit a distorted octahedral geometry, where the coordination sites are occupied by two nitrogen atoms of one tmphen ligand, two bridging cyanide groups and two oxygen atoms of a DMF and a CH3OH molecule. The eight-coordinated W centres adopt a distorted square antiprismatic geometry, where three cyanide groups bridge to adjacent three Mn atoms and the others are terminal. As a result, the W1 and Mn1 atoms are connected alternatively by cyanide groups to form a tetranuclear 12-atom rhombic metallacycle, Mn12W12(CN)4, with the W1 and Mn1 centres located at the vertexes and the cyanide groups forming the sides. Similarly, another rhombic cycle, Mn32W22(CN)4, is also formed by the connection of W2 and Mn3 atoms through cyanide anions. The Mn2 atoms further link alternatively adjacent circles through –CN–Mn2—NC– linkages, generating a 3,2-chain structure parallel to [1 0 1]. Adjacent chains are linked by π-π interactions involving the phenanthroline rings systems, with centroid-to-centroid distances of 3.763 (3) and 3.620 (2) Å. The structural feature observed in the title compound has been also found in other octacyanometalate-based materials (Li et al., 2002; Li et al., 2003; Withers et al., 2007).

Related literature top

For general background to octacyanometalate-based compounds, see: Nowicka et al. (2012); Sieklucka et al. (2011). For related structures, see: Li et al. (2002, 2003); Withers et al. (2007). For the synthesis of octacyanotungstate(V), see: Bok et al. (1975).

Experimental top

The title compound was prepared at room temperature by slow diffusion of a CH3OH/DMF solution (1:1 v/v) containing [HN(n-C4H9)3[W(CN)8] (0.05 mmol) (Bok et al., 1975) and MnCl2·4H2O (0.15 mmol) into a methanol solution of tmphen (0.1 mmol). After about two weeks, brown block crystals were obtained on slow evaporation of the solvent.

Refinement top

The two independent water molecule are disordered over three sets of sites with refined occupancy ratios of 0.310 (9):0.275 (9):0.415 (9) for one molecule and 0.335 (9):0.288 (9):0.377 (9) for the other molecule. The hydroxy and water H atoms were located in a difference Fourier map and refined as riding [O—H = 0.85 Å, U(H) = 1.5Ueq(O) for water H atoms; O—H = 0.97 Å, U(H) = 1.2Ueq(O) for hydroxy H atoms]. All other H atoms were calculated at idealized positions and included in the refinement in a riding mode, with C–H = 0.93-0.97 Å and with U(H) = 1.2Ueq(C) or 1.5Ueq(C) for methyl H atoms.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound with displacement ellipsoids drawn at the 30% probability level. H atoms and disordered water molecules are omitted for clarity. Symmetry code: (i) -x, -y + 2, -z; (ii) -x + 1, -y + 2, -z + 1.
[Figure 2] Fig. 2. The 3,2-chain structure of the title compound. H atoms, coordinated methanol and DMF ligands, terminal cyanide groups, and water molecules are omitted for clarity.
Poly[[tetra-µ-cyanido-κ8C:N-dodeca-cyanido-κ12C-tris(N,N-dimethylformamide-κO)tris(methanol-κO)tris(3,4,7,8-tetramethyl-1,10-phenanthroline-κ2N,N')trimanganese(II)ditungstate(V)] dihydrate] top
Crystal data top
[Mn3W2(CN)16(C16H16N2)3(C3H7NO)3(CH4O)3]·2H2OZ = 2
Mr = 2009.20F(000) = 2006
Triclinic, P1Dx = 1.418 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 15.5038 (17) ÅCell parameters from 9991 reflections
b = 16.4958 (18) Åθ = 2.5–27.3°
c = 21.4067 (13) ŵ = 2.89 mm1
α = 70.008 (2)°T = 291 K
β = 82.663 (3)°Block, brown
γ = 66.129 (2)°0.24 × 0.20 × 0.18 mm
V = 4704.4 (8) Å3
Data collection top
Bruker SMART APEXII
diffractometer
17934 independent reflections
Radiation source: sealed tube14773 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.016
phi and ω scansθmax = 26.0°, θmin = 1.4°
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
h = 1818
Tmin = 0.50, Tmax = 0.60k = 2020
35664 measured reflectionsl = 2626
Refinement top
Refinement on F22 restraints
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.046H-atom parameters constrained
wR(F2) = 0.117 w = 1/[σ2(Fo2) + (0.07P)2 + 1.88P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.002
17934 reflectionsΔρmax = 1.38 e Å3
1078 parametersΔρmin = 0.92 e Å3
Crystal data top
[Mn3W2(CN)16(C16H16N2)3(C3H7NO)3(CH4O)3]·2H2Oγ = 66.129 (2)°
Mr = 2009.20V = 4704.4 (8) Å3
Triclinic, P1Z = 2
a = 15.5038 (17) ÅMo Kα radiation
b = 16.4958 (18) ŵ = 2.89 mm1
c = 21.4067 (13) ÅT = 291 K
α = 70.008 (2)°0.24 × 0.20 × 0.18 mm
β = 82.663 (3)°
Data collection top
Bruker SMART APEXII
diffractometer
17934 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
14773 reflections with I > 2σ(I)
Tmin = 0.50, Tmax = 0.60Rint = 0.016
35664 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0462 restraints
wR(F2) = 0.117H-atom parameters constrained
S = 1.05Δρmax = 1.38 e Å3
17934 reflectionsΔρmin = 0.92 e Å3
1078 parameters
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
xyzUiso*/UeqOcc. (<1)
C10.1521 (3)0.8254 (4)0.0296 (3)0.0359 (12)
C20.3782 (3)0.7348 (3)0.1466 (2)0.0310 (11)
C30.3539 (4)0.9040 (4)0.0708 (3)0.0429 (13)
C40.1993 (4)0.8160 (3)0.1541 (3)0.0354 (12)
C50.2751 (4)0.8947 (4)0.0439 (3)0.0396 (13)
C60.2926 (4)0.6808 (4)0.0810 (3)0.0389 (12)
C70.4185 (4)0.7582 (4)0.0219 (3)0.0457 (14)
C80.1791 (4)0.9644 (4)0.0506 (3)0.0357 (12)
C90.5504 (3)0.7187 (4)0.3507 (2)0.0358 (12)
C100.6241 (4)0.8491 (4)0.4541 (3)0.0377 (12)
C110.5441 (3)0.7372 (3)0.5347 (2)0.0301 (11)
C120.6920 (4)0.7414 (3)0.3850 (3)0.0344 (11)
C130.6214 (3)0.6260 (4)0.4708 (3)0.0342 (11)
C140.4292 (4)0.7417 (3)0.4451 (2)0.0325 (11)
C150.5299 (3)0.8921 (4)0.3384 (3)0.0351 (11)
C160.4397 (4)0.8921 (4)0.4495 (3)0.0351 (11)
C170.2202 (4)0.8318 (4)0.0874 (3)0.0410 (13)
H170.24510.88930.08000.049*
C180.2813 (4)0.8061 (4)0.1164 (3)0.0391 (12)
C190.2414 (4)0.7213 (4)0.1306 (2)0.0404 (13)
C200.1446 (4)0.6640 (4)0.1161 (2)0.0373 (12)
C210.0995 (4)0.5785 (4)0.1275 (3)0.0459 (14)
H210.13310.55790.14720.055*
C220.0097 (4)0.5256 (4)0.1110 (3)0.0471 (14)
H220.01830.47100.12230.057*
C230.0461 (4)0.5482 (3)0.0768 (2)0.0350 (11)
C240.1423 (4)0.4928 (3)0.0594 (3)0.0403 (12)
C250.1892 (4)0.5245 (4)0.0273 (3)0.0394 (12)
C260.1365 (4)0.6138 (4)0.0141 (3)0.0395 (12)
H260.16680.63420.00840.047*
C270.0028 (3)0.6366 (4)0.0651 (3)0.0355 (11)
C280.0929 (4)0.6942 (4)0.0845 (2)0.0373 (12)
C290.3840 (4)0.8691 (4)0.1280 (3)0.0490 (15)
H29A0.39840.89180.17460.073*
H29B0.39720.92100.11250.073*
H29C0.42180.83460.10420.073*
C300.2991 (4)0.6941 (4)0.1652 (3)0.0499 (15)
H30A0.36470.73250.16360.075*
H30B0.28920.62950.14340.075*
H30C0.28000.70290.21070.075*
C310.1926 (4)0.4025 (4)0.0733 (3)0.0524 (15)
H31A0.21130.41460.11900.079*
H31B0.15140.36950.06480.079*
H31C0.24750.36510.04510.079*
C320.2883 (4)0.4722 (4)0.0034 (3)0.0499 (15)
H32A0.29640.41020.02480.075*
H32B0.30320.50390.02130.075*
H32C0.32950.46880.04070.075*
C330.5531 (4)0.4911 (4)0.1545 (3)0.0396 (13)
H330.49110.53460.14780.048*
C340.5804 (4)0.4181 (4)0.1271 (3)0.0458 (14)
C350.6719 (4)0.3496 (4)0.1393 (3)0.0416 (13)
C360.7347 (4)0.3573 (4)0.1769 (2)0.0355 (11)
C370.8265 (4)0.2962 (4)0.1901 (3)0.0396 (12)
H370.84780.24570.17410.048*
C380.8898 (4)0.3034 (4)0.2252 (3)0.0468 (14)
H380.95180.26020.23150.056*
C390.8564 (3)0.3825 (4)0.2529 (2)0.0345 (11)
C400.9163 (4)0.3951 (4)0.2905 (3)0.0391 (12)
C410.8787 (4)0.4701 (4)0.3136 (2)0.0357 (11)
C420.7823 (4)0.5281 (4)0.3031 (3)0.0384 (12)
H420.75660.57590.32190.046*
C430.7631 (3)0.4459 (3)0.2411 (2)0.0314 (11)
C440.7007 (3)0.4341 (3)0.2017 (2)0.0321 (11)
C450.5094 (4)0.4124 (4)0.0877 (3)0.0490 (15)
H45A0.53290.41330.04390.073*
H45B0.45070.46480.08470.073*
H45C0.49980.35540.10980.073*
C460.7036 (4)0.2726 (4)0.1097 (3)0.0451 (14)
H46A0.69780.21800.14190.068*
H46B0.76830.25850.09670.068*
H46C0.66520.29190.07140.068*
C471.0180 (4)0.3308 (4)0.3010 (3)0.0486 (15)
H47A1.05080.35600.31950.073*
H47B1.04540.32460.25920.073*
H47C1.02320.27050.33100.073*
C480.9371 (4)0.4916 (4)0.3514 (3)0.0416 (13)
H48A0.98000.43430.38070.062*
H48B0.89650.52990.37700.062*
H48C0.97210.52440.32080.062*
C490.9022 (4)0.7775 (3)0.4635 (2)0.0354 (11)
H490.85320.77900.44170.042*
C500.9923 (3)0.7061 (4)0.4656 (2)0.0333 (11)
C511.0648 (4)0.7027 (4)0.4979 (3)0.0420 (13)
C521.0468 (2)0.7745 (2)0.52851 (17)0.0415 (13)
C531.11751 (17)0.7759 (2)0.56158 (18)0.0437 (14)
H531.17820.73040.56440.052*
C541.09746 (18)0.8453 (2)0.59036 (16)0.0388 (12)
H541.14480.84620.61250.047*
C551.0067 (2)0.9133 (2)0.58607 (16)0.0323 (11)
C590.93601 (15)0.9120 (2)0.55300 (17)0.0328 (11)
C600.95606 (18)0.8426 (2)0.52422 (17)0.0356 (12)
C560.9821 (4)0.9883 (4)0.6154 (3)0.0386 (12)
C570.8944 (3)1.0571 (4)0.6045 (2)0.0335 (11)
C580.8272 (4)1.0498 (4)0.5679 (3)0.0371 (12)
H580.76721.09700.56040.045*
C611.0044 (4)0.6359 (4)0.4306 (3)0.0426 (13)
H61A1.05070.63880.39640.064*
H61B0.94530.65070.41110.064*
H61C1.02490.57400.46230.064*
C621.1618 (4)0.6307 (4)0.4991 (3)0.0408 (13)
H62A1.16180.59000.47600.061*
H62B1.18190.59480.54430.061*
H62C1.20410.66090.47770.061*
C631.0555 (4)0.9869 (4)0.6562 (3)0.0439 (13)
H63A1.04611.04990.65150.066*
H63B1.11730.95600.64100.066*
H63C1.04980.95380.70210.066*
C640.8631 (4)1.1363 (4)0.6303 (3)0.0445 (13)
H64A0.84871.11610.67660.067*
H64B0.80791.18540.60620.067*
H64C0.91251.15910.62500.067*
C650.1503 (5)0.7056 (5)0.2047 (4)0.070 (2)
H65A0.18560.70610.17070.106*
H65B0.18910.71080.24290.106*
H65C0.09570.64810.21680.106*
C660.1321 (6)0.8402 (5)0.2256 (3)0.069 (2)
H66A0.07170.83770.23420.103*
H66B0.15880.81420.26670.103*
H66C0.17330.90410.20520.103*
C670.0962 (5)0.8135 (4)0.1114 (3)0.0544 (16)
H670.09010.87090.09490.065*
C680.0515 (3)0.9458 (4)0.1466 (3)0.0381 (12)
H68A0.00141.00330.14920.057*
H68B0.08160.95080.18900.057*
H68C0.09560.93390.11370.057*
C690.6410 (5)0.8428 (4)0.0452 (3)0.0575 (17)
H69A0.70800.82420.03950.086*
H69B0.60910.89970.01030.086*
H69C0.62280.79450.04350.086*
C700.6049 (4)0.9500 (4)0.1132 (3)0.0505 (15)
H70A0.58560.95360.15690.076*
H70B0.55810.99900.08120.076*
H70C0.66420.95690.10330.076*
C710.6026 (4)0.7898 (4)0.1670 (3)0.0419 (13)
H710.58320.80490.20600.050*
C720.5586 (6)0.4704 (6)0.3905 (3)0.076 (2)
H72A0.61390.41410.39480.114*
H72B0.51040.45580.41930.114*
H72C0.57390.51390.40270.114*
C730.5550 (4)1.1644 (4)0.2629 (3)0.0566 (16)
H73A0.51531.20810.28490.085*
H73B0.52161.12930.25730.085*
H73C0.57201.19770.22010.085*
C740.7089 (4)1.0296 (5)0.2743 (3)0.0578 (17)
H74A0.77201.01440.28720.087*
H74B0.70291.05490.22670.087*
H74C0.69540.97410.28950.087*
C750.6556 (4)1.0941 (4)0.3687 (3)0.0411 (13)
H750.60651.13480.38660.049*
C760.6534 (4)0.8406 (4)0.6353 (3)0.0442 (13)
H76A0.62570.89460.64980.066*
H76B0.66500.78500.67310.066*
H76C0.61090.84350.60490.066*
Mn10.03069 (5)0.81206 (5)0.02729 (3)0.02748 (16)
Mn20.56980 (5)0.60947 (5)0.24169 (3)0.02728 (16)
Mn30.74155 (5)0.94644 (5)0.50428 (4)0.02783 (16)
N10.0866 (3)0.8243 (3)0.0120 (2)0.0336 (9)
N20.4310 (3)0.6892 (3)0.1902 (2)0.0380 (10)
N30.3941 (3)0.9495 (3)0.0763 (2)0.0441 (11)
N40.1516 (3)0.8172 (3)0.1998 (2)0.0467 (12)
N50.2666 (3)0.9319 (3)0.0990 (2)0.0387 (10)
N60.2984 (3)0.6095 (3)0.0904 (2)0.0465 (12)
N70.4890 (3)0.7237 (3)0.0028 (2)0.0462 (11)
N80.1279 (3)1.0414 (3)0.04165 (19)0.0287 (9)
N90.5485 (3)0.6895 (3)0.3092 (2)0.0389 (10)
N100.6631 (3)0.8854 (3)0.4688 (2)0.0378 (10)
N110.5381 (3)0.7220 (3)0.5902 (2)0.0447 (11)
N120.7669 (3)0.7213 (3)0.3624 (2)0.0446 (11)
N130.6539 (3)0.5467 (3)0.4967 (2)0.0537 (14)
N140.3619 (3)0.7270 (3)0.4550 (2)0.0439 (11)
N150.5146 (3)0.9545 (3)0.2906 (2)0.0469 (12)
N160.3781 (3)0.9527 (3)0.4608 (2)0.0380 (10)
N170.1326 (3)0.7784 (3)0.0715 (2)0.0351 (10)
N180.0488 (3)0.6653 (3)0.0330 (2)0.0369 (10)
N190.6115 (3)0.5017 (3)0.1901 (2)0.0362 (10)
N200.7263 (3)0.5166 (3)0.26685 (19)0.0342 (10)
N210.8853 (3)0.8417 (3)0.4914 (2)0.0353 (10)
N220.8461 (3)0.9800 (3)0.5443 (2)0.0334 (9)
N230.1205 (4)0.7845 (4)0.1795 (3)0.0560 (13)
N240.6151 (3)0.8585 (3)0.1104 (2)0.0462 (11)
N250.6421 (3)1.0991 (3)0.3038 (2)0.0452 (11)
O10.0828 (3)0.7703 (3)0.07290 (18)0.0450 (9)
O20.0193 (2)0.8697 (2)0.12824 (16)0.0358 (8)
H2B0.03150.88890.15900.043*
O30.6160 (3)0.7103 (2)0.16782 (18)0.0409 (9)
O40.5258 (3)0.5103 (3)0.32424 (17)0.0441 (9)
H4B0.53670.45820.30870.053*
O50.7262 (2)1.0410 (3)0.40470 (17)0.0413 (9)
O60.7408 (3)0.8384 (3)0.60266 (18)0.0430 (9)
H6B0.77900.84220.63330.052*
O1W0.1213 (11)0.5827 (10)0.2403 (7)0.068 (5)0.310 (9)
H1WA0.07230.57300.23750.101*0.310 (9)
H1WC0.11610.60250.27290.101*0.310 (9)
O2W0.6638 (11)0.2913 (11)0.3608 (8)0.060 (5)0.275 (9)
H2WA0.66800.24730.39700.090*0.275 (9)
H2WB0.69540.26850.33100.090*0.275 (9)
O3W0.6552 (8)0.6032 (7)0.7210 (5)0.061 (4)0.415 (9)
H3WA0.70980.57930.73850.092*0.415 (9)
H3WC0.61570.59280.75080.092*0.415 (9)
O4W0.8202 (8)0.6538 (7)0.6107 (5)0.042 (3)0.335 (9)
H4WD0.77950.64030.63810.050*0.335 (9)
H4WB0.86480.60380.60820.062*0.335 (9)
O5W0.2852 (10)0.6327 (9)0.3382 (6)0.049 (4)0.288 (9)
H5WA0.25580.61540.31780.073*0.288 (9)
H5WB0.24570.67250.35540.073*0.288 (9)
O6W0.7496 (6)1.0023 (5)0.7488 (4)0.028 (3)0.377 (9)
H6WB0.69091.01400.74920.042*0.377 (9)
H6WC0.77350.99040.71340.042*0.377 (9)
W10.28113 (2)0.82252 (2)0.06363 (2)0.03084 (7)
W20.55316 (2)0.77498 (2)0.42800 (2)0.02667 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.025 (3)0.046 (3)0.041 (3)0.011 (2)0.006 (2)0.020 (2)
C20.026 (2)0.039 (3)0.031 (3)0.015 (2)0.006 (2)0.010 (2)
C30.037 (3)0.037 (3)0.048 (3)0.015 (2)0.020 (3)0.003 (3)
C40.033 (3)0.034 (3)0.029 (3)0.006 (2)0.013 (2)0.003 (2)
C50.049 (3)0.035 (3)0.032 (3)0.011 (3)0.008 (2)0.009 (2)
C60.032 (3)0.040 (3)0.046 (3)0.012 (2)0.009 (2)0.015 (3)
C70.028 (3)0.068 (4)0.037 (3)0.012 (3)0.012 (2)0.016 (3)
C80.036 (3)0.034 (3)0.041 (3)0.020 (2)0.004 (2)0.008 (2)
C90.033 (3)0.044 (3)0.033 (3)0.010 (2)0.002 (2)0.020 (2)
C100.042 (3)0.036 (3)0.038 (3)0.021 (2)0.008 (2)0.005 (2)
C110.031 (3)0.033 (3)0.030 (3)0.014 (2)0.005 (2)0.012 (2)
C120.031 (3)0.037 (3)0.034 (3)0.011 (2)0.007 (2)0.011 (2)
C130.028 (3)0.035 (3)0.035 (3)0.006 (2)0.006 (2)0.015 (2)
C140.032 (3)0.025 (2)0.033 (3)0.003 (2)0.013 (2)0.006 (2)
C150.030 (3)0.035 (3)0.034 (3)0.008 (2)0.002 (2)0.009 (2)
C160.031 (3)0.034 (3)0.039 (3)0.007 (2)0.008 (2)0.014 (2)
C170.027 (3)0.044 (3)0.054 (4)0.014 (2)0.003 (2)0.017 (3)
C180.034 (3)0.055 (3)0.032 (3)0.027 (3)0.002 (2)0.006 (2)
C190.052 (3)0.048 (3)0.028 (3)0.030 (3)0.007 (2)0.004 (2)
C200.048 (3)0.049 (3)0.023 (3)0.026 (3)0.001 (2)0.013 (2)
C210.059 (4)0.057 (4)0.039 (3)0.036 (3)0.002 (3)0.021 (3)
C220.053 (4)0.051 (3)0.039 (3)0.021 (3)0.005 (3)0.013 (3)
C230.043 (3)0.033 (3)0.032 (3)0.017 (2)0.004 (2)0.012 (2)
C240.048 (3)0.027 (3)0.040 (3)0.009 (2)0.005 (2)0.009 (2)
C250.043 (3)0.038 (3)0.032 (3)0.013 (2)0.005 (2)0.006 (2)
C260.039 (3)0.036 (3)0.040 (3)0.016 (2)0.009 (2)0.002 (2)
C270.030 (3)0.038 (3)0.034 (3)0.011 (2)0.006 (2)0.011 (2)
C280.038 (3)0.051 (3)0.033 (3)0.023 (3)0.003 (2)0.020 (2)
C290.032 (3)0.071 (4)0.034 (3)0.017 (3)0.001 (2)0.008 (3)
C300.045 (3)0.065 (4)0.047 (4)0.027 (3)0.002 (3)0.019 (3)
C310.064 (4)0.037 (3)0.052 (4)0.019 (3)0.019 (3)0.017 (3)
C320.049 (3)0.040 (3)0.055 (4)0.022 (3)0.007 (3)0.001 (3)
C330.033 (3)0.041 (3)0.047 (3)0.009 (2)0.017 (2)0.016 (3)
C340.049 (3)0.037 (3)0.045 (3)0.005 (3)0.019 (3)0.013 (3)
C350.057 (4)0.030 (3)0.033 (3)0.014 (3)0.017 (3)0.001 (2)
C360.038 (3)0.037 (3)0.032 (3)0.012 (2)0.004 (2)0.015 (2)
C370.036 (3)0.044 (3)0.032 (3)0.014 (3)0.012 (2)0.010 (2)
C380.033 (3)0.049 (3)0.058 (4)0.014 (3)0.007 (3)0.021 (3)
C390.032 (3)0.044 (3)0.029 (3)0.021 (2)0.002 (2)0.007 (2)
C400.033 (3)0.046 (3)0.034 (3)0.011 (2)0.006 (2)0.010 (2)
C410.036 (3)0.041 (3)0.029 (3)0.020 (2)0.002 (2)0.004 (2)
C420.035 (3)0.049 (3)0.035 (3)0.019 (2)0.003 (2)0.013 (2)
C430.030 (3)0.032 (3)0.035 (3)0.016 (2)0.005 (2)0.011 (2)
C440.031 (3)0.030 (3)0.031 (3)0.010 (2)0.000 (2)0.007 (2)
C450.048 (3)0.038 (3)0.067 (4)0.012 (3)0.019 (3)0.023 (3)
C460.049 (3)0.034 (3)0.056 (4)0.012 (3)0.012 (3)0.019 (3)
C470.041 (3)0.037 (3)0.050 (4)0.003 (3)0.016 (3)0.001 (3)
C480.030 (3)0.052 (3)0.039 (3)0.018 (3)0.007 (2)0.005 (3)
C490.032 (3)0.036 (3)0.030 (3)0.006 (2)0.002 (2)0.009 (2)
C500.025 (2)0.043 (3)0.029 (3)0.015 (2)0.019 (2)0.013 (2)
C510.026 (3)0.052 (3)0.037 (3)0.007 (2)0.005 (2)0.012 (3)
C520.033 (3)0.027 (3)0.049 (3)0.003 (2)0.010 (2)0.001 (2)
C530.035 (3)0.042 (3)0.040 (3)0.006 (2)0.011 (2)0.018 (3)
C540.023 (3)0.047 (3)0.037 (3)0.005 (2)0.007 (2)0.011 (2)
C550.023 (2)0.044 (3)0.022 (2)0.009 (2)0.0001 (19)0.007 (2)
C590.018 (2)0.039 (3)0.037 (3)0.009 (2)0.008 (2)0.013 (2)
C600.027 (3)0.042 (3)0.040 (3)0.016 (2)0.001 (2)0.012 (2)
C560.037 (3)0.035 (3)0.035 (3)0.009 (2)0.006 (2)0.005 (2)
C570.035 (3)0.038 (3)0.030 (3)0.018 (2)0.011 (2)0.013 (2)
C580.036 (3)0.043 (3)0.039 (3)0.018 (2)0.005 (2)0.020 (2)
C610.041 (3)0.040 (3)0.043 (3)0.010 (3)0.008 (2)0.018 (3)
C620.032 (3)0.043 (3)0.035 (3)0.006 (2)0.010 (2)0.011 (2)
C630.043 (3)0.048 (3)0.043 (3)0.024 (3)0.000 (3)0.009 (3)
C640.035 (3)0.054 (3)0.047 (3)0.014 (3)0.003 (2)0.025 (3)
C650.083 (5)0.069 (5)0.070 (5)0.047 (4)0.004 (4)0.015 (4)
C660.092 (6)0.077 (5)0.050 (4)0.043 (4)0.023 (4)0.030 (4)
C670.082 (5)0.048 (3)0.036 (3)0.029 (3)0.010 (3)0.015 (3)
C680.025 (3)0.045 (3)0.042 (3)0.012 (2)0.007 (2)0.011 (3)
C690.058 (4)0.054 (4)0.047 (4)0.013 (3)0.016 (3)0.016 (3)
C700.042 (3)0.062 (4)0.054 (4)0.029 (3)0.011 (3)0.018 (3)
C710.042 (3)0.053 (4)0.030 (3)0.016 (3)0.001 (2)0.014 (3)
C720.097 (6)0.085 (5)0.038 (4)0.050 (5)0.012 (4)0.012 (4)
C730.037 (3)0.057 (4)0.053 (4)0.007 (3)0.007 (3)0.002 (3)
C740.054 (4)0.062 (4)0.038 (3)0.001 (3)0.003 (3)0.021 (3)
C750.031 (3)0.050 (3)0.042 (3)0.013 (3)0.012 (2)0.022 (3)
C760.045 (3)0.067 (4)0.029 (3)0.029 (3)0.002 (2)0.017 (3)
Mn10.0281 (4)0.0317 (4)0.0259 (4)0.0128 (3)0.0077 (3)0.0086 (3)
Mn20.0288 (4)0.0307 (4)0.0254 (4)0.0115 (3)0.0082 (3)0.0098 (3)
Mn30.0246 (4)0.0327 (4)0.0286 (4)0.0085 (3)0.0055 (3)0.0136 (3)
N10.025 (2)0.040 (2)0.035 (2)0.0101 (18)0.0076 (18)0.0114 (19)
N20.031 (2)0.042 (3)0.036 (2)0.010 (2)0.006 (2)0.009 (2)
N30.038 (3)0.045 (3)0.047 (3)0.019 (2)0.007 (2)0.006 (2)
N40.046 (3)0.042 (3)0.031 (3)0.001 (2)0.002 (2)0.005 (2)
N50.037 (2)0.039 (3)0.033 (3)0.015 (2)0.002 (2)0.004 (2)
N60.042 (3)0.038 (3)0.056 (3)0.006 (2)0.017 (2)0.017 (2)
N70.035 (3)0.057 (3)0.048 (3)0.016 (2)0.007 (2)0.024 (2)
N80.031 (2)0.034 (2)0.026 (2)0.0136 (19)0.0083 (17)0.0106 (18)
N90.038 (2)0.059 (3)0.024 (2)0.018 (2)0.0104 (18)0.024 (2)
N100.030 (2)0.036 (2)0.054 (3)0.0117 (19)0.007 (2)0.021 (2)
N110.042 (3)0.055 (3)0.027 (3)0.025 (2)0.000 (2)0.008 (2)
N120.036 (3)0.054 (3)0.036 (3)0.013 (2)0.002 (2)0.009 (2)
N130.041 (3)0.047 (3)0.043 (3)0.018 (2)0.008 (2)0.018 (2)
N140.036 (3)0.046 (3)0.046 (3)0.017 (2)0.003 (2)0.010 (2)
N150.051 (3)0.040 (3)0.037 (3)0.014 (2)0.003 (2)0.000 (2)
N160.030 (2)0.037 (2)0.045 (3)0.005 (2)0.0068 (19)0.017 (2)
N170.031 (2)0.043 (2)0.036 (2)0.017 (2)0.0013 (18)0.015 (2)
N180.038 (3)0.037 (2)0.035 (2)0.011 (2)0.0029 (19)0.015 (2)
N190.035 (2)0.041 (2)0.038 (2)0.0100 (19)0.0023 (19)0.023 (2)
N200.031 (2)0.046 (3)0.023 (2)0.0094 (19)0.0031 (17)0.0163 (19)
N210.018 (2)0.043 (2)0.043 (3)0.0078 (18)0.0027 (18)0.019 (2)
N220.0155 (19)0.036 (2)0.044 (3)0.0046 (17)0.0061 (17)0.012 (2)
N230.073 (4)0.056 (3)0.046 (3)0.032 (3)0.014 (3)0.020 (3)
N240.045 (3)0.044 (3)0.044 (3)0.013 (2)0.006 (2)0.015 (2)
N250.036 (3)0.049 (3)0.043 (3)0.013 (2)0.004 (2)0.013 (2)
O10.048 (2)0.056 (2)0.036 (2)0.025 (2)0.0110 (17)0.0169 (19)
O20.0311 (19)0.046 (2)0.0271 (18)0.0147 (16)0.0024 (14)0.0084 (16)
O30.045 (2)0.036 (2)0.040 (2)0.0166 (17)0.0114 (17)0.0139 (17)
O40.043 (2)0.048 (2)0.0297 (19)0.0183 (18)0.0015 (16)0.0025 (17)
O50.032 (2)0.049 (2)0.033 (2)0.0107 (17)0.0025 (16)0.0085 (17)
O60.042 (2)0.045 (2)0.038 (2)0.0149 (18)0.0020 (17)0.0115 (17)
O1W0.075 (11)0.060 (10)0.062 (10)0.031 (8)0.007 (8)0.010 (8)
O2W0.066 (11)0.059 (10)0.056 (10)0.021 (8)0.019 (8)0.030 (8)
O3W0.072 (8)0.070 (8)0.044 (6)0.031 (6)0.017 (5)0.023 (5)
O4W0.040 (7)0.032 (6)0.043 (7)0.009 (5)0.017 (5)0.001 (5)
O5W0.052 (9)0.042 (8)0.038 (8)0.007 (7)0.021 (6)0.017 (6)
O6W0.027 (5)0.030 (5)0.027 (5)0.016 (4)0.012 (4)0.001 (4)
W10.02969 (12)0.03556 (12)0.02926 (12)0.01160 (9)0.00575 (8)0.01186 (9)
W20.02480 (11)0.03159 (11)0.02509 (11)0.00796 (8)0.00767 (8)0.01161 (8)
Geometric parameters (Å, º) top
C1—N11.138 (6)C51—C621.489 (7)
C1—W12.192 (5)C52—C531.3900
C2—N21.152 (6)C52—C601.3900
C2—W12.162 (5)C53—C541.3900
C3—N31.193 (6)C53—H530.9300
C3—W12.125 (5)C54—C551.3900
C4—N41.149 (7)C54—H540.9300
C4—W12.172 (6)C55—C591.3900
C5—N51.125 (6)C55—C561.468 (6)
C5—W12.193 (5)C59—N221.377 (4)
C6—N61.091 (6)C59—C601.3900
C6—W12.173 (6)C60—N211.384 (4)
C7—N71.107 (7)C56—C571.358 (7)
C7—W12.190 (6)C56—C631.510 (7)
C8—N81.156 (6)C57—C581.444 (7)
C8—W12.174 (5)C57—C641.470 (7)
C9—N91.154 (6)C58—N221.323 (6)
C9—W22.168 (5)C58—H580.9300
C10—N101.137 (6)C61—H61A0.9600
C10—W22.175 (5)C61—H61B0.9600
C11—N111.127 (6)C61—H61C0.9600
C11—W22.154 (5)C62—H62A0.9600
C12—N121.160 (6)C62—H62B0.9600
C12—W22.161 (5)C62—H62C0.9600
C13—N131.147 (7)C63—H63A0.9600
C13—W22.145 (5)C63—H63B0.9600
C14—N141.143 (6)C63—H63C0.9600
C14—W22.160 (5)C64—H64A0.9600
C15—N151.145 (6)C64—H64B0.9600
C15—W22.149 (5)C64—H64C0.9600
C16—N161.142 (6)C65—N231.463 (8)
C16—W22.166 (5)C65—H65A0.9600
C17—N171.296 (6)C65—H65B0.9600
C17—C181.455 (7)C65—H65C0.9600
C17—H170.9300C66—N231.514 (8)
C18—C191.406 (8)C66—H66A0.9600
C18—C291.503 (7)C66—H66B0.9600
C19—C201.419 (8)C66—H66C0.9600
C19—C301.507 (7)C67—O11.212 (6)
C20—C211.390 (8)C67—N231.424 (7)
C20—C281.427 (7)C67—H670.9300
C21—C221.324 (8)C68—O21.449 (6)
C21—H210.9300C68—H68A0.9600
C22—C231.425 (7)C68—H68B0.9600
C22—H220.9300C68—H68C0.9600
C23—C241.417 (7)C69—N241.482 (7)
C23—C271.434 (7)C69—H69A0.9600
C24—C251.397 (7)C69—H69B0.9600
C24—C311.490 (7)C69—H69C0.9600
C25—C261.472 (7)C70—N241.473 (7)
C25—C321.482 (7)C70—H70A0.9600
C26—N181.305 (6)C70—H70B0.9600
C26—H260.9300C70—H70C0.9600
C27—N181.350 (6)C71—O31.237 (6)
C27—C281.422 (7)C71—N241.403 (7)
C28—N171.384 (6)C71—H710.9300
C29—H29A0.9600C72—O41.407 (7)
C29—H29B0.9600C72—H72A0.9600
C29—H29C0.9600C72—H72B0.9600
C30—H30A0.9600C72—H72C0.9600
C30—H30B0.9600C73—N251.494 (7)
C30—H30C0.9600C73—H73A0.9600
C31—H31A0.9600C73—H73B0.9600
C31—H31B0.9600C73—H73C0.9600
C31—H31C0.9600C74—N251.467 (7)
C32—H32A0.9600C74—H74A0.9600
C32—H32B0.9600C74—H74B0.9600
C32—H32C0.9600C74—H74C0.9600
C33—N191.351 (6)C75—O51.241 (6)
C33—C341.409 (7)C75—N251.401 (7)
C33—H330.9300C75—H750.9300
C34—C351.397 (8)C76—O61.437 (6)
C34—C451.518 (7)C76—H76A0.9600
C35—C361.406 (7)C76—H76B0.9600
C35—C461.491 (7)C76—H76C0.9600
C36—C371.367 (7)Mn1—O12.174 (4)
C36—C441.419 (7)Mn1—N12.203 (4)
C37—C381.372 (8)Mn1—N8i2.207 (4)
C37—H370.9300Mn1—O22.222 (3)
C38—C391.492 (7)Mn1—N182.269 (4)
C38—H380.9300Mn1—N172.270 (4)
C39—C431.392 (7)Mn2—O32.158 (4)
C39—C401.420 (7)Mn2—N92.185 (4)
C40—C411.369 (7)Mn2—O42.210 (3)
C40—C471.496 (7)Mn2—N22.213 (4)
C41—C421.408 (7)Mn2—N192.242 (4)
C41—C481.497 (7)Mn2—N202.299 (4)
C42—N201.341 (6)Mn3—O52.142 (4)
C42—H420.9300Mn3—N16ii2.183 (4)
C43—N201.345 (6)Mn3—N102.196 (4)
C43—C441.470 (7)Mn3—O62.248 (4)
C44—N191.368 (6)Mn3—N222.253 (4)
C45—H45A0.9600Mn3—N212.254 (4)
C45—H45B0.9600N8—Mn1i2.208 (4)
C45—H45C0.9600N16—Mn3ii2.183 (4)
C46—H46A0.9600O2—H2B0.9700
C46—H46B0.9600O4—H4B0.9700
C46—H46C0.9600O6—H6B0.9700
C47—H47A0.9600O1W—H1WA0.8500
C47—H47B0.9600O1W—H1WC0.8500
C47—H47C0.9600O2W—H2WA0.8500
C48—H48A0.9600O2W—H2WB0.8500
C48—H48B0.9600O3W—H3WA0.8501
C48—H48C0.9600O3W—H3WC0.8501
C49—N211.309 (6)O4W—H4WD0.8500
C49—C501.410 (7)O4W—H4WB0.8500
C49—H490.9300O5W—H5WA0.8500
C50—C511.366 (7)O5W—H5WB0.8501
C50—C611.521 (7)O6W—H6WB0.8500
C51—C521.459 (6)O6W—H6WC0.8500
N1—C1—W1178.0 (5)H66A—C66—H66C109.5
N2—C2—W1178.6 (5)H66B—C66—H66C109.5
N3—C3—W1178.5 (5)O1—C67—N23125.9 (6)
N4—C4—W1175.9 (4)O1—C67—H67117.0
N5—C5—W1175.8 (5)N23—C67—H67117.0
N6—C6—W1179.3 (5)O2—C68—H68A109.5
N7—C7—W1177.7 (5)O2—C68—H68B109.5
N8—C8—W1176.7 (5)H68A—C68—H68B109.5
N9—C9—W2179.4 (5)O2—C68—H68C109.5
N10—C10—W2178.0 (5)H68A—C68—H68C109.5
N11—C11—W2176.5 (4)H68B—C68—H68C109.5
N12—C12—W2178.4 (5)N24—C69—H69A109.5
N13—C13—W2175.7 (5)N24—C69—H69B109.5
N14—C14—W2177.3 (5)H69A—C69—H69B109.5
N15—C15—W2177.7 (5)N24—C69—H69C109.5
N16—C16—W2178.0 (4)H69A—C69—H69C109.5
N17—C17—C18123.2 (5)H69B—C69—H69C109.5
N17—C17—H17118.4N24—C70—H70A109.5
C18—C17—H17118.4N24—C70—H70B109.5
C19—C18—C17117.8 (5)H70A—C70—H70B109.5
C19—C18—C29122.9 (5)N24—C70—H70C109.5
C17—C18—C29119.2 (5)H70A—C70—H70C109.5
C18—C19—C20119.6 (4)H70B—C70—H70C109.5
C18—C19—C30120.4 (5)O3—C71—N24123.4 (5)
C20—C19—C30119.9 (5)O3—C71—H71118.3
C21—C20—C19123.6 (5)N24—C71—H71118.3
C21—C20—C28118.7 (5)O4—C72—H72A109.5
C19—C20—C28117.5 (5)O4—C72—H72B109.5
C22—C21—C20121.7 (5)H72A—C72—H72B109.5
C22—C21—H21119.1O4—C72—H72C109.5
C20—C21—H21119.1H72A—C72—H72C109.5
C21—C22—C23123.3 (6)H72B—C72—H72C109.5
C21—C22—H22118.3N25—C73—H73A109.5
C23—C22—H22118.3N25—C73—H73B109.5
C24—C23—C22123.9 (5)H73A—C73—H73B109.5
C24—C23—C27119.1 (4)N25—C73—H73C109.5
C22—C23—C27116.7 (5)H73A—C73—H73C109.5
C25—C24—C23117.9 (5)H73B—C73—H73C109.5
C25—C24—C31120.4 (5)N25—C74—H74A109.5
C23—C24—C31121.7 (5)N25—C74—H74B109.5
C24—C25—C26118.5 (5)H74A—C74—H74B109.5
C24—C25—C32124.1 (5)N25—C74—H74C109.5
C26—C25—C32117.3 (5)H74A—C74—H74C109.5
N18—C26—C25122.4 (5)H74B—C74—H74C109.5
N18—C26—H26118.8O5—C75—N25126.7 (5)
C25—C26—H26118.8O5—C75—H75116.7
N18—C27—C28118.6 (5)N25—C75—H75116.7
N18—C27—C23121.8 (5)O6—C76—H76A109.5
C28—C27—C23119.5 (5)O6—C76—H76B109.5
N17—C28—C27117.8 (4)H76A—C76—H76B109.5
N17—C28—C20122.3 (5)O6—C76—H76C109.5
C27—C28—C20119.9 (5)H76A—C76—H76C109.5
C18—C29—H29A109.5H76B—C76—H76C109.5
C18—C29—H29B109.5O1—Mn1—N190.22 (15)
H29A—C29—H29B109.5O1—Mn1—N8i90.16 (15)
C18—C29—H29C109.5N1—Mn1—N8i94.90 (14)
H29A—C29—H29C109.5O1—Mn1—O2173.74 (14)
H29B—C29—H29C109.5N1—Mn1—O287.02 (14)
C19—C30—H30A109.5N8i—Mn1—O284.48 (14)
C19—C30—H30B109.5O1—Mn1—N1896.27 (15)
H30A—C30—H30B109.5N1—Mn1—N1897.25 (15)
C19—C30—H30C109.5N8i—Mn1—N18166.21 (14)
H30A—C30—H30C109.5O2—Mn1—N1889.66 (14)
H30B—C30—H30C109.5O1—Mn1—N1793.12 (15)
C24—C31—H31A109.5N1—Mn1—N17170.42 (16)
C24—C31—H31B109.5N8i—Mn1—N1794.07 (14)
H31A—C31—H31B109.5O2—Mn1—N1790.49 (14)
C24—C31—H31C109.5N18—Mn1—N1773.47 (15)
H31A—C31—H31C109.5O3—Mn2—N988.29 (15)
H31B—C31—H31C109.5O3—Mn2—O4174.77 (14)
C25—C32—H32A109.5N9—Mn2—O486.86 (16)
C25—C32—H32B109.5O3—Mn2—N286.21 (15)
H32A—C32—H32B109.5N9—Mn2—N297.96 (16)
C25—C32—H32C109.5O4—Mn2—N296.40 (15)
H32A—C32—H32C109.5O3—Mn2—N1998.63 (15)
H32B—C32—H32C109.5N9—Mn2—N19167.68 (17)
N19—C33—C34123.9 (5)O4—Mn2—N1985.80 (16)
N19—C33—H33118.0N2—Mn2—N1992.69 (15)
C34—C33—H33118.0O3—Mn2—N2087.44 (15)
C35—C34—C33118.8 (5)N9—Mn2—N2097.24 (15)
C35—C34—C45121.2 (5)O4—Mn2—N2091.22 (14)
C33—C34—C45119.9 (5)N2—Mn2—N20163.32 (15)
C34—C35—C36119.1 (5)N19—Mn2—N2073.05 (14)
C34—C35—C46120.1 (5)O5—Mn3—N16ii92.69 (15)
C36—C35—C46120.7 (5)O5—Mn3—N1085.73 (16)
C37—C36—C35124.2 (5)N16ii—Mn3—N1098.12 (16)
C37—C36—C44118.1 (5)O5—Mn3—O6169.83 (14)
C35—C36—C44117.7 (5)N16ii—Mn3—O687.63 (15)
C36—C37—C38125.3 (5)N10—Mn3—O684.16 (16)
C36—C37—H37117.4O5—Mn3—N2299.45 (15)
C38—C37—H37117.4N16ii—Mn3—N2292.17 (15)
C37—C38—C39118.3 (5)N10—Mn3—N22168.27 (15)
C37—C38—H38120.9O6—Mn3—N2290.68 (15)
C39—C38—H38120.9O5—Mn3—N2196.53 (15)
C43—C39—C40119.2 (5)N16ii—Mn3—N21164.33 (15)
C43—C39—C38118.4 (4)N10—Mn3—N2195.18 (15)
C40—C39—C38122.4 (5)O6—Mn3—N2185.51 (15)
C41—C40—C39117.7 (5)N22—Mn3—N2173.86 (15)
C41—C40—C47121.9 (5)C1—N1—Mn1174.2 (4)
C39—C40—C47120.3 (5)C2—N2—Mn2157.7 (4)
C40—C41—C42119.8 (5)C8—N8—Mn1i178.5 (4)
C40—C41—C48121.8 (5)C9—N9—Mn2168.2 (4)
C42—C41—C48118.4 (5)C10—N10—Mn3175.6 (4)
N20—C42—C41122.1 (5)C16—N16—Mn3ii171.7 (5)
N20—C42—H42118.9C17—N17—C28119.5 (4)
C41—C42—H42118.9C17—N17—Mn1126.1 (4)
N20—C43—C39122.1 (4)C28—N17—Mn1114.4 (3)
N20—C43—C44118.1 (4)C26—N18—C27120.1 (4)
C39—C43—C44119.7 (4)C26—N18—Mn1124.4 (4)
N19—C44—C36123.9 (4)C27—N18—Mn1115.2 (3)
N19—C44—C43115.9 (4)C33—N19—C44116.4 (4)
C36—C44—C43120.2 (4)C33—N19—Mn2125.7 (4)
C34—C45—H45A109.5C44—N19—Mn2117.4 (3)
C34—C45—H45B109.5C42—N20—C43118.8 (4)
H45A—C45—H45B109.5C42—N20—Mn2126.0 (3)
C34—C45—H45C109.5C43—N20—Mn2115.2 (3)
H45A—C45—H45C109.5C49—N21—C60121.0 (4)
H45B—C45—H45C109.5C49—N21—Mn3125.5 (3)
C35—C46—H46A109.5C60—N21—Mn3113.0 (3)
C35—C46—H46B109.5C58—N22—C59118.2 (4)
H46A—C46—H46B109.5C58—N22—Mn3126.9 (3)
C35—C46—H46C109.5C59—N22—Mn3114.2 (3)
H46A—C46—H46C109.5C67—N23—C65119.4 (5)
H46B—C46—H46C109.5C67—N23—C66123.1 (5)
C40—C47—H47A109.5C65—N23—C66116.8 (5)
C40—C47—H47B109.5C71—N24—C70121.4 (5)
H47A—C47—H47B109.5C71—N24—C69122.3 (5)
C40—C47—H47C109.5C70—N24—C69116.3 (5)
H47A—C47—H47C109.5C75—N25—C74121.0 (5)
H47B—C47—H47C109.5C75—N25—C73124.2 (5)
C41—C48—H48A109.5C74—N25—C73114.2 (5)
C41—C48—H48B109.5C67—O1—Mn1123.5 (4)
H48A—C48—H48B109.5C68—O2—Mn1123.7 (3)
C41—C48—H48C109.5C68—O2—H2B106.5
H48A—C48—H48C109.5Mn1—O2—H2B106.5
H48B—C48—H48C109.5C71—O3—Mn2127.4 (3)
N21—C49—C50122.2 (5)C72—O4—Mn2127.3 (4)
N21—C49—H49118.9C72—O4—H4B105.9
C50—C49—H49118.9Mn2—O4—H4B105.2
C51—C50—C49119.5 (5)C75—O5—Mn3131.7 (3)
C51—C50—C61122.7 (5)C76—O6—Mn3120.4 (3)
C49—C50—C61117.8 (5)C76—O6—H6B106.9
C50—C51—C52118.7 (4)Mn3—O6—H6B107.0
C50—C51—C62121.3 (5)H1WA—O1W—H1WC109.5
C52—C51—C62120.0 (4)H2WA—O2W—H2WB109.5
C53—C52—C60120.0H3WA—O3W—H3WC109.5
C53—C52—C51121.7 (3)H4WD—O4W—H4WB109.5
C60—C52—C51118.3 (3)H5WA—O5W—H5WB109.5
C54—C53—C52120.0H6WB—O6W—H6WC109.5
C54—C53—H53120.0C3—W1—C274.74 (18)
C52—C53—H53120.0C3—W1—C4101.0 (2)
C53—C54—C55120.0C2—W1—C472.33 (18)
C53—C54—H54120.0C3—W1—C6144.32 (19)
C55—C54—H54120.0C2—W1—C674.05 (18)
C59—C55—C54120.0C4—W1—C685.6 (2)
C59—C55—C56118.0 (3)C3—W1—C871.71 (19)
C54—C55—C56122.0 (3)C2—W1—C8126.01 (19)
N22—C59—C55122.6 (3)C4—W1—C874.08 (19)
N22—C59—C60117.3 (3)C6—W1—C8142.57 (18)
C55—C59—C60120.0C3—W1—C778.1 (2)
N21—C60—C59119.6 (3)C2—W1—C773.20 (19)
N21—C60—C52120.4 (3)C4—W1—C7144.41 (19)
C59—C60—C52120.0C6—W1—C776.7 (2)
C57—C56—C55119.0 (4)C8—W1—C7135.9 (2)
C57—C56—C63122.0 (5)C3—W1—C1145.66 (19)
C55—C56—C63119.0 (4)C2—W1—C1135.46 (19)
C56—C57—C58118.1 (5)C4—W1—C179.52 (19)
C56—C57—C64123.4 (5)C6—W1—C169.94 (19)
C58—C57—C64118.4 (5)C8—W1—C175.59 (18)
N22—C58—C57123.9 (5)C7—W1—C1121.09 (19)
N22—C58—H58118.0C3—W1—C586.2 (2)
C57—C58—H58118.0C2—W1—C5142.7 (2)
C50—C61—H61A109.5C4—W1—C5143.97 (19)
C50—C61—H61B109.5C6—W1—C5109.0 (2)
H61A—C61—H61B109.5C8—W1—C574.9 (2)
C50—C61—H61C109.5C7—W1—C571.6 (2)
H61A—C61—H61C109.5C1—W1—C575.3 (2)
H61B—C61—H61C109.5C13—W2—C15145.16 (19)
C51—C62—H62A109.5C13—W2—C1170.73 (18)
C51—C62—H62B109.5C15—W2—C11143.17 (18)
H62A—C62—H62B109.5C13—W2—C1481.68 (18)
C51—C62—H62C109.5C15—W2—C14108.03 (18)
H62A—C62—H62C109.5C11—W2—C1479.00 (18)
H62B—C62—H62C109.5C13—W2—C1275.69 (19)
C56—C63—H63A109.5C15—W2—C1278.12 (19)
C56—C63—H63B109.5C11—W2—C12117.69 (18)
H63A—C63—H63B109.5C14—W2—C12144.27 (18)
C56—C63—H63C109.5C13—W2—C16139.58 (19)
H63A—C63—H63C109.5C15—W2—C1674.13 (19)
H63B—C63—H63C109.5C11—W2—C1673.61 (19)
C57—C64—H64A109.5C14—W2—C1673.39 (18)
C57—C64—H64B109.5C12—W2—C16139.65 (19)
H64A—C64—H64B109.5C13—W2—C974.57 (19)
C57—C64—H64C109.5C15—W2—C976.4 (2)
H64A—C64—H64C109.5C11—W2—C9138.27 (19)
H64B—C64—H64C109.5C14—W2—C973.65 (19)
N23—C65—H65A109.5C12—W2—C973.89 (18)
N23—C65—H65B109.5C16—W2—C9125.42 (18)
H65A—C65—H65B109.5C13—W2—C10112.44 (19)
N23—C65—H65C109.5C15—W2—C1079.54 (19)
H65A—C65—H65C109.5C11—W2—C1075.67 (18)
H65B—C65—H65C109.5C14—W2—C10144.3 (2)
N23—C66—H66A109.5C12—W2—C1071.0 (2)
N23—C66—H66B109.5C16—W2—C1075.58 (19)
H66A—C66—H66B109.5C9—W2—C10140.6 (2)
N23—C66—H66C109.5
N17—C17—C18—C193.2 (8)C49—C50—C51—C62177.7 (5)
N17—C17—C18—C29175.0 (5)C61—C50—C51—C621.8 (8)
C17—C18—C19—C200.5 (7)C50—C51—C52—C53179.3 (4)
C29—C18—C19—C20177.7 (5)C62—C51—C52—C532.6 (6)
C17—C18—C19—C30175.5 (5)C50—C51—C52—C601.0 (6)
C29—C18—C19—C306.3 (8)C62—C51—C52—C60177.7 (4)
C18—C19—C20—C21179.0 (5)C60—C52—C53—C540.0
C30—C19—C20—C215.0 (8)C51—C52—C53—C54179.7 (4)
C18—C19—C20—C282.7 (7)C52—C53—C54—C550.0
C30—C19—C20—C28178.7 (5)C53—C54—C55—C590.0
C19—C20—C21—C22177.6 (5)C53—C54—C55—C56179.7 (4)
C28—C20—C21—C221.3 (8)C54—C55—C59—N22176.7 (4)
C20—C21—C22—C234.1 (9)C56—C55—C59—N223.0 (4)
C21—C22—C23—C24179.4 (6)C54—C55—C59—C600.0
C21—C22—C23—C275.0 (8)C56—C55—C59—C60179.7 (4)
C22—C23—C24—C25178.4 (5)N22—C59—C60—N213.1 (4)
C27—C23—C24—C254.1 (8)C55—C59—C60—N21180.0 (4)
C22—C23—C24—C312.6 (8)N22—C59—C60—C52176.9 (4)
C27—C23—C24—C31177.0 (5)C55—C59—C60—C520.0
C23—C24—C25—C260.6 (8)C53—C52—C60—N21180.0 (4)
C31—C24—C25—C26179.6 (5)C51—C52—C60—N210.3 (4)
C23—C24—C25—C32177.2 (5)C53—C52—C60—C590.0
C31—C24—C25—C321.8 (9)C51—C52—C60—C59179.7 (4)
C24—C25—C26—N182.0 (8)C59—C55—C56—C575.4 (6)
C32—C25—C26—N18180.0 (5)C54—C55—C56—C57174.4 (4)
C24—C23—C27—N185.4 (8)C59—C55—C56—C63175.1 (4)
C22—C23—C27—N18179.9 (5)C54—C55—C56—C635.1 (6)
C24—C23—C27—C28177.9 (5)C55—C56—C57—C583.9 (7)
C22—C23—C27—C283.1 (7)C63—C56—C57—C58176.6 (5)
N18—C27—C28—N172.4 (7)C55—C56—C57—C64178.7 (5)
C23—C27—C28—N17179.2 (5)C63—C56—C57—C640.8 (8)
N18—C27—C28—C20177.5 (5)C56—C57—C58—N220.1 (8)
C23—C27—C28—C200.7 (8)C64—C57—C58—N22177.5 (5)
C21—C20—C28—N17179.8 (5)C18—C17—N17—C282.4 (8)
C19—C20—C28—N173.7 (8)C18—C17—N17—Mn1179.3 (4)
C21—C20—C28—C270.3 (8)C27—C28—N17—C17178.7 (5)
C19—C20—C28—C27176.2 (5)C20—C28—N17—C171.2 (8)
N19—C33—C34—C352.9 (9)C27—C28—N17—Mn14.1 (6)
N19—C33—C34—C45179.9 (5)C20—C28—N17—Mn1176.1 (4)
C33—C34—C35—C361.9 (9)C25—C26—N18—C270.9 (8)
C45—C34—C35—C36179.0 (5)C25—C26—N18—Mn1171.3 (4)
C33—C34—C35—C46178.6 (5)C28—C27—N18—C26179.5 (5)
C45—C34—C35—C464.2 (9)C23—C27—N18—C262.8 (8)
C34—C35—C36—C37177.8 (5)C28—C27—N18—Mn17.6 (6)
C46—C35—C36—C371.1 (9)C23—C27—N18—Mn1175.7 (4)
C34—C35—C36—C441.2 (8)C34—C33—N19—C442.9 (8)
C46—C35—C36—C44177.9 (5)C34—C33—N19—Mn2175.0 (4)
C35—C36—C37—C38178.3 (5)C36—C44—N19—C332.1 (8)
C44—C36—C37—C380.7 (8)C43—C44—N19—C33179.3 (5)
C36—C37—C38—C391.6 (9)C36—C44—N19—Mn2174.8 (4)
C37—C38—C39—C430.9 (8)C43—C44—N19—Mn26.6 (6)
C37—C38—C39—C40179.2 (5)C41—C42—N20—C431.7 (8)
C43—C39—C40—C410.1 (8)C41—C42—N20—Mn2177.1 (4)
C38—C39—C40—C41179.8 (5)C39—C43—N20—C422.3 (7)
C43—C39—C40—C47176.9 (5)C44—C43—N20—C42179.8 (4)
C38—C39—C40—C473.0 (8)C39—C43—N20—Mn2178.8 (4)
C39—C40—C41—C423.9 (8)C44—C43—N20—Mn21.3 (6)
C47—C40—C41—C42179.4 (5)C50—C49—N21—C600.3 (8)
C39—C40—C41—C48177.6 (5)C50—C49—N21—Mn3170.8 (4)
C47—C40—C41—C480.8 (8)C59—C60—N21—C49179.7 (4)
C40—C41—C42—N204.9 (8)C52—C60—N21—C490.3 (6)
C48—C41—C42—N20176.5 (5)C59—C60—N21—Mn38.2 (4)
C40—C39—C43—N203.1 (8)C52—C60—N21—Mn3171.80 (18)
C38—C39—C43—N20176.9 (5)C57—C58—N22—C592.6 (7)
C40—C39—C43—C44179.4 (5)C57—C58—N22—Mn3167.4 (4)
C38—C39—C43—C440.5 (7)C55—C59—N22—C580.9 (6)
C37—C36—C44—N19177.8 (5)C60—C59—N22—C58175.9 (4)
C35—C36—C44—N191.3 (8)C55—C59—N22—Mn3170.35 (18)
C37—C36—C44—C430.8 (7)C60—C59—N22—Mn312.8 (4)
C35—C36—C44—C43179.8 (5)O1—C67—N23—C6512.7 (10)
N20—C43—C44—N195.2 (7)O1—C67—N23—C66177.2 (7)
C39—C43—C44—N19177.3 (5)O3—C71—N24—C70175.5 (5)
N20—C43—C44—C36176.2 (5)O3—C71—N24—C693.2 (8)
C39—C43—C44—C361.4 (7)O5—C75—N25—C748.6 (9)
N21—C49—C50—C510.4 (8)O5—C75—N25—C73179.7 (5)
N21—C49—C50—C61179.1 (5)N23—C67—O1—Mn1172.9 (5)
C49—C50—C51—C521.0 (7)N24—C71—O3—Mn2164.4 (4)
C61—C50—C51—C52178.4 (4)N25—C75—O5—Mn3127.9 (5)
Symmetry codes: (i) x, y+2, z; (ii) x+1, y+2, z+1.

Experimental details

Crystal data
Chemical formula[Mn3W2(CN)16(C16H16N2)3(C3H7NO)3(CH4O)3]·2H2O
Mr2009.20
Crystal system, space groupTriclinic, P1
Temperature (K)291
a, b, c (Å)15.5038 (17), 16.4958 (18), 21.4067 (13)
α, β, γ (°)70.008 (2), 82.663 (3), 66.129 (2)
V3)4704.4 (8)
Z2
Radiation typeMo Kα
µ (mm1)2.89
Crystal size (mm)0.24 × 0.20 × 0.18
Data collection
DiffractometerBruker SMART APEXII
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2004)
Tmin, Tmax0.50, 0.60
No. of measured, independent and
observed [I > 2σ(I)] reflections
35664, 17934, 14773
Rint0.016
(sin θ/λ)max1)0.617
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.046, 0.117, 1.05
No. of reflections17934
No. of parameters1078
No. of restraints2
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.38, 0.92

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL2013 (Sheldrick, 2008), DIAMOND (Brandenburg, 2006), SHELXTL (Sheldrick, 2008).

 

References

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First citationBrandenburg, K. (2006). DIAMOND. Crystal Impact GbR, Bonn, Germany.
First citationBruker (2004). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
First citationLi, D. F., Gao, S., Zheng, L. M. & Tang, W. X. (2002). J. Chem. Soc. Dalton Trans. pp. 2805–2806.  Web of Science CSD CrossRef
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First citationNowicka, B., Korzeniak, T., Stefańczyk, O., Pinkowicz, D., Chorąży, S., Podgajny, R. & Sieklucka, B. (2012). Coord. Chem. Rev. 256, 1946–1971.  Web of Science CrossRef CAS
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First citationSieklucka, B., Podgajny, R., Korzeniak, T., Nowicka, B., Pinkowicz, D. & Kozieł, M. (2011). Eur. J. Inorg. Chem. pp. 305–326.  Web of Science CrossRef
First citationWithers, J. R., Li, D. F., Triplet, J., Ruschman, C., Parkin, S., Wang, G. B., Yee, G. T. & Holmes, S. M. (2007). Polyhedron, 26, 2353–2366.  Web of Science CSD CrossRef CAS

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Volume 70| Part 5| May 2014| Pages m170-m171
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