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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 8| August 2011| Pages m1041-m1042
doi:10.1107/S160053681102602X

Di-μ-acetato-bis­­(di­methyl­formamide)­penta­kis­(μ-N,2-dioxido­benzene-1-car­boximidato)tetra­kis­(1-ethyl­imidazole)­penta­manganese(III)­manganese(II)–di­ethyl ether–di­methyl­foramide–methanol–water (1/1/1/1/0.12)

Benjamin R. Tigyer,a Matthias Zellerb and Curtis M. Zaleskia*

aDepartment of Chemistry, Shippensburg University, 1871 Old Main Dr., Shippensburg, PA 17257, USA, and bDepartment of Chemistry, Youngstown State University, 1 University Plaza, Youngstown, OH 44555, USA
*Correspondence e-mail: cmzaleski@ship.edu

(Received 24 May 2011; accepted 30 June 2011; online 9 July 2011)

The title compound [Mn6(C7H4NO3)5(CH3CO2)2(C5H8N2)4(C3H7NO)2]·(C2H5)2O·C3H7NO·CH3OH·0.12H2O, abbreviated as MnII(OAc)2[15-MCMnIII(N)shi-5](EtIm)4(DMF)2·diethyl ether·DMF·MeOH·0.12H2O (where −OAc is acetate, MC is metallacrown, shi3− is salicylhydroximate, EtIM is n-ethylimidazole, DMF is N,N-dimethylformamide, and MeOH is methanol) contains five MnIII ions as members of the metallacrown ring and an MnII ion bound in the central cavity. The central MnII ion is seven-coordinate with a distorted face-capped trigonal–prismatic geometry. The five MnIII ions of the metallacrown ring are six-coordinate with distorted octa­hedral geometries. The configuration of the MnIII ions about the metallacrown ring follow a ΔΛΔPP pattern, with P representing planar. The four 1-ethyl­imidazole ligands are bound to four different MnIII ions. A diethyl ether solvent mol­ecule was found to be disordered over two mutually exclusive sites with an occupancy ratio of 0.568 (7):0.432 (7). A methanol solvent mol­ecule was found to be disordered over two mutually exclusive sites by being hydrogen bonded either to a dimethyl­formamide solvent mol­ecule (major occupancy component) or to an O atom of the main mol­ecule (minor occupancy component). The occupancy ratio refined to 0.678 (11):0.322 (11). Associated with the minor component is a partially occupied water mol­ecule [total occupancy 0.124 (15)].

Related literature

For a general review of metallacrowns, see: Mezei et al. (2007[Mezei, G., Zaleski, C. M. & Pecoraro, V. L. (2007). Chem. Rev. 107, 4933-5003.]); Pecoraro et al. (1997[Pecoraro, V. L., Stemmler, A. J., Gibney, B. R., Bodwin, J. J., Wang, H., Kampf, J. W. & Barwinski, A. (1997). Progress in Inorganic Chemistry, edited by K. D. Karlin, pp. 83-177. New York: Wiley.]). For related MnII[15-MCMnIIIN(shi)-5)] structures, see: Kessissoglou et al. (1994[Kessissoglou, D. P., Kampf, J. & Pecoraro, V. L. (1994). Polyhedron, 13, 1379-1391.]); Dendrinou-Samara et al. (2002[Dendrinou-Samara, C., Alevizopoulou, L., Iordanidis, L., Samaras, E. & Kessissoglou, D. P. (2002). J. Inorg. Biochem. 89, 89-96.], 2005[Dendrinou-Samara, C., Papadopoulos, A. N., Malamatari, D. A., Tarushi, A., Raptopoulou, C. P., Terzis, A., Samaras, E. & Kessissoglou, D. P. (2005). J. Inorg. Biochem. 99, 864-875.]); Emerich et al. (2010[Emerich, B., Smith, M., Zeller, M. & Zaleski, C. M. (2010). J. Chem. Crystallogr. 40, 769-777.]). For an explanation of how to calculate the s/h ratio, see: Stiefel & Brown (1972[Stiefel, E. I. & Brown, G. F. (1972). Inorg. Chem. 11, 434-436.]). For the preparation of {MnII(OAc)2[12-MCMnIIIN(shi)-4](DMF)6}·2DMF, see: Lah & Pecoraro (1989[Lah, M. S. & Pecoraro, V. L. (1989). J. Am. Chem. Soc. 111, 7258-7259.]).

[Scheme 1]

Experimental

Crystal data

  • [Mn6(C7H4NO3)5(C2H3O2)2(C5H8N2)4(C3H7NO)2]·C4H10O·C3H7NO·CH4O·0.12H2O

  • Mr = 1910.51

  • Triclinic, [P \overline 1]

  • a = 12.604 (2) Å

  • b = 17.188 (3) Å

  • c = 20.990 (4) Å

  • α = 103.564 (3)°

  • β = 97.322 (3)°

  • γ = 107.658 (3)°

  • V = 4114.2 (13) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 0.98 mm−1

  • T = 100 K

  • 0.35 × 0.29 × 0.13 mm
Data collection

  • Bruker SMART APEX CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.563, Tmax = 0.746

  • 49270 measured reflections

  • 18692 independent reflections

  • 14786 reflections with I > 2σ(I)

  • Rint = 0.046
Refinement

  • R[F2 > 2σ(F2)] = 0.059

  • wR(F2) = 0.148

  • S = 1.07

  • 18692 reflections

  • 1143 parameters

  • 53 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 1.53 e Å−3

  • Δρmin = −0.76 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O24—H24A⋯O22 0.84 2.09 2.876 (7) 156
O24B—H24B⋯O19 0.84 2.15 2.98 (2) 170
O25—H25A⋯O24B 0.84 (2) 2.35 (2) 3.05 (4) 140 (6)
O25—H25B⋯O22 0.84 (2) 1.99 (2) 2.776 (17) 156 (4)

Data collection: APEX2 (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL, Mercury (Macrae et al., 2006[Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P., Taylor, R., Towler, M. & van de Streek, J. (2006). J. Appl. Cryst. 39, 453-457.]) and ORTEP-3 (Farrugia, 1997[Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.]); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053681102602X/jj2091sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S160053681102602X/jj2091Isup2.hkl

checkCIF report


Comment top

Metallacrowns (MCs) are a versatile class of inorganic molecules that serve both as structural and functional analogues to crown ethers (Mezei et al., 2007; Pecoraro et al., 1997). In addition to mimicking crown ethers, MCs have other potential uses such as single-molecule magnets, MRI contrast agents, and catalysts (Mezei et al., 2007). The naming scheme for MCs is similar to that of crown ethers. For example, 15-MC-5 indicates that the ring size of the MC consists of 15 atoms and that there are 5 oxygen atoms capable of binding a metal ion in the central cavity. A complete naming scheme can be found in the review by Pecoraro et al. (1997). Manganese-based 15-MC-5 structures were the first 15-MC-5 compounds reported (Kessissoglou et al., 1994), and some of these molecules have shown antibacterial activity (Dendrinou-Samara et al., 2002; Dendrinou-Samara et al., 2005).

Herein we report the synthesis, IR data, and the single-crystal X-ray structure of the title compound,[Mn6(C7H4NO3)5(C5N2H8)4(C3H7NO)2(C2H3O2)2].(C2H5)2O.C3H7NO.CH3OH.0.12H2O, 1, abbreviated as MnII(OAc)2[15-MCMnIIIN(shi)-5](EtIm)4(DMF)2.Diethyl ether.DMF.MeOH.0.12H2O (where -OAc is acetate, MC is metallacrown, shi3- is salicylhydroximate, EtIM is n-ethylimidazole, DMF is N,N-dimethylformamide, and MeOH is methanol). The single-crystal X-ray structure of a related molecule, MnII(OAc)2[15-MCMnIIIN(shi)-5](Im)3(EtOH)3 (where Im is imidazole and EtOH is ethanol), has previously been reported by Emerich et al. (2010).

Compound 1 is a non-planar molecule, which is typical of MnII[15-MCMnIII-5] structures (Fig. 1–5; Farrugia, 1997). The structure consists of a [MnIII—N—O]5 repeat unit around the MC ring, and the MC binds a MnII in the central cavity (Fig. 1). The positive charge of the five MnIII ions and the one MnII ion are counterbalanced by the five shi3- ligands and two acetate anions. Mn1 is located in the central cavity and is seven-coordinate with distorted face-capped trigonal prismatic geometry (Fig. 2). The geometry assignment is based on the calculated azimuthal angle (Φ). In an ideal face-capped octahedron Φ = 60°, while in an ideal face-capped trigonal prism Φ = 0°. To calculate the Φ angle, the centers of opposite triangular faces made by the donor oxygen atoms (O1, O13, and O18; O7, O10, and O17) were defined using the program Mercury (Macrae et al., 2006), and then twist angles between atoms on opposite faces through the centroids were calculated (Fig. 3). The calculated Φ angles of 9.77°, 12.78°, and 15.95° indicate the geometry approaches more that of face-capped trigonal prismatic. Another parameter that indicates the geometry is the s/h ratio (Stiefel and Brown, 1972). In an ideal octahedron the s/h ratio is 1.22, while in an ideal trigonal prism the s/h ratio is 1.00. Defining the distance between the centroids in Fig. 3 as h, the average s/h ratio for 1 is 1.00 ± 0.10. Thus both the Φ angle and the s/h ratio support a distorted face-capped trigonal prismatic geometry. The assignment of 2+ for Mn1 is supported by an average bond distance of 2.24 Å. The ring Mn (2–6) are assigned a 3+ oxidation state. This is supported by the average bond distance, and the observation of a Jahn-Teller axis for each ring Mn, which is typical for a high spin d4 cation. The average bond distances for Mn2, Mn3, Mn4, Mn5, and Mn6 are 2.03 Å, 2.03 Å, 2.03 Å, 2.05 Å, and 2.09 Å, respectively. Each MnIII is six-coordinate with a distorted octahedral geometry (Fig. 4). It should be noted that Mn6 has one long interaction with an acetate oxygen atom (Mn6—O18, 2.684 (3) Å) that is needed to complete the octahedral geometry. The coordination about the MnIII ions can also be described by their configurations. Mn2 has a propeller configuration with Δ absolute stereochemistry. Mn3 and Mn4 do not adopt a propeller configuration, but instead two shi3- ligands are trans to each other. Thus, Mn3 and Mn4 adopt a planar (P) configuration. Mn5 has a propeller configuration with Δ absolute stereochemistry, and Mn6 has a propeller configuration with Λ absolute stereochemistry. Starting with Mn5, the configuration pattern for the MnIII ions about the MC ring is ΔΛΔPP. In addition, Mn2, Mn4, Mn5, and Mn6 bind n-ethylimidazole ligands, which are directed to the periphery of the molecule. Lastly, a disordered diethyl ether molecule, a disordered methanol molecule, a dimethylformamide molecule, and a partially occupied water molecule (0.124 (15)) are located in the lattice.

Related literature top

For a general review of metallacrowns, see: Mezei et al. (2007); Pecoraro et al. (1997). For related MnII[15-MCMnIIIN(shi)-5)] structures, see: Kessissoglou et al. (1994); Dendrinou-Samara et al. (2002, 2005); Emerich et al. (2010). For an explanation on how to calculate the s/h ratio, see: Stiefel & Brown (1972). For the preparation of {MnII(OAc)2[12-MCMnIIIN(shi)-4](DMF)6}.2DMF, see: Lah & Pecoraro (1989).

Experimental top

Manganese(II) acetate tetrahydrate (99+%) and N,N-dimethylformamide (ACS grade) were purchased from Acros Organics, salicylhydroxamic acid (H3shi, 99%) was purchased from Alfa Aesar, n-ethylimidazole (98%) was purchased from TCI America, methanol (HPLC grade) was purchased from Fisher Scientific, and absolute diethyl ether was purchased from EMD Chemicals. All reagents were used as received and without further purification.

The compound {MnII(OAc)2[12-MCMnIIIN(shi)-4](DMF)6}.2DMF was prepared as previously reported (Lah & Pecoraro, 1989), and dark brown crystals were isolated and dried. Then 0.1 mmol of the {MnII(OAc)2[12-MCMnIIIN(shi)-4](DMF)6}.2DMF compound was dissolved in 20 ml of a 50:50 mixture of methanol and DMF. The resulting mixture was a dark brown color. Then 25 µL of n-ethylimidazole was added to this solution, and the solution was stirred for 5 minutes. The resulting dark brown solution was filtered and no precipitate was recovered. Diffusion of diethyl ether into the filtrate at approximately 277 K (4 °C) resulted in dark brown cube-like crystals after 9 days. The percent yield was 22% based on the {MnII(OAc)2[12-MCMnIIIN(shi)-4](DMF)6}.2DMF starting material. Elemental analysis for the dried material (accounting for the loss of the diethyl ether lattice solvent) C69H83.24Mn6N16O23.12 [FW = 1836.28 g/mol] found % (calculated); C 45.59 (45.13); H 4.44 (4.57); N 12.37 (12.20).

Refinement top

A solvent diethyl ether molecule was found to be disordered over two mutually exclusive sites. The molecules were restrained to have similar geometries and equivalent atoms were constrained to have identical ADPs. The occupancy ratio refined to 0.568 (7) to 0.432 (7). A solvent methanol molecule was found to be disordered over two mutually exclusive sites by being hydrogen bonded either to a solvent DMF molecule (major moiety) or to an oxygen atom of the main molecule (minor moiety). The two molecules were restrained to have similar C—O distances. The occupancy ratio refined to 0.678 (11) to 0.322 (11). Associated with the minor moiety is a partially occupied water molecule (total occupancy: 0.124 (15). This position of the water oxygen atom and of its H atoms was restrained based on hydrogen bonding considerations. It was also restrained to be approximately isotropic. The carbon atoms of one ethyl group (C48, C49) showed signs of unresolved disorder and were restrained to be approximately isotropic.

Hydrogen atoms were placed in calculated positions with C—H = 0.95 (aromatic), 0.98 (methyl) and 0.99 Å (methylene) and were refined with Uĩso~(H) = 1.5 Ueq(C) for methyl H atoms and 1.2 Ueq(C) for methylene and aromatic moieties.

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008), Mercury (Macrae et al., 2006) and ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Single-crystal X-ray structure of MnII(OAc)2[15-MCMnIIIN(shi)-5](EtIm)4(DMF)2.Diethyl ether.DMF.MeOH.0.14H2O (1). The thermal ellipsoid plot of 1 is at a 50% probability level. All atoms composing the MC ring are labeled. Hydrogen atoms and the lattice solvent molecules have been omitted for clarity. Color scheme for all figures: purple - MnII and MnIII, red - oxygen, blue - nitrogen, and gray - carbon.
[Figure 2] Fig. 2. Side (left) and top (right) views of the first coordination sphere about Mn1 (2+ oxidation state) of 1 with face-capped trigonal prismatic geometry. The thermal ellipsoid plots are at a 50% probability level.
[Figure 3] Fig. 3. Side (left) and top (right) views of the first coordination sphere about Mn1 of 1 indicating how the azimuthal angle (Φ) was defined and calculated with the program Mercury (Macrae et al., 2006). The thermal ellipsoid plots are at a 50% probability level.
[Figure 4] Fig. 4. First coordination sphere about each MnIII ion of 1. a) Mn2 with Δ configuration b) Mn3 with planar configuration c) Mn4 with planar configuration d) Mn5 with Δ configuration and e) Mn6 with Λ configuration. The thermal ellipsoid plots are at a 50% probability level. Hydrogen atoms have been omitted for clarity.
[Figure 5] Fig. 5. Packing diagram of 1 along the a axis. The thermal ellipsoid plot is at a 50% probability level. Hydrogen atoms have been omitted for clarity.
Di-µ-acetato-bis(dimethylformamide)pentakis(µ- N,2-dioxidobenzene-1-carboximidato)tetrakis(1- ethylimidazole)pentamanganese(III)manganese(II)– diethyl ether–dimethylforamide–methanol–water (1/1/1/1/0.12) top
Crystal data top
[Mn6(C7H4NO3)5(C2H3O2)2(C5H8N2)4(C3H7NO)2]·C4H10O·C3H7NO·CH4O·0.12H2OZ = 2
Mr = 1910.51F(000) = 1972.1
Triclinic, P1Dx = 1.542 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.604 (2) ÅCell parameters from 1712 reflections
b = 17.188 (3) Åθ = 2.7–30.2°
c = 20.990 (4) ŵ = 0.98 mm−1
α = 103.564 (3)°T = 100 K
β = 97.322 (3)°Plate, black
γ = 107.658 (3)°0.35 × 0.29 × 0.13 mm
V = 4114.2 (13) Å3
Data collection top
Bruker SMART APEX CCD
diffractometer		18692 independent reflections
Radiation source: fine-focus sealed tube14786 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
ω scansθmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan
(SADABS; Bruker, 2009)		h = −16→16
Tmin = 0.563, Tmax = 0.746k = −22→22
49270 measured reflectionsl = −27→27
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)] = 0.059Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.148H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.0581P)2 + 8.5964P]
where P = (Fo2 + 2Fc2)/3
18692 reflections(Δ/σ)max = 0.002
1143 parametersΔρmax = 1.53 e Å−3
53 restraintsΔρmin = −0.76 e Å−3
5 constraints
Crystal data top
[Mn6(C7H4NO3)5(C2H3O2)2(C5H8N2)4(C3H7NO)2]·C4H10O·C3H7NO·CH4O·0.12H2Oγ = 107.658 (3)°
Mr = 1910.51V = 4114.2 (13) Å3
Triclinic, P1Z = 2
a = 12.604 (2) ÅMo Kα radiation
b = 17.188 (3) ŵ = 0.98 mm−1
c = 20.990 (4) ÅT = 100 K
α = 103.564 (3)°0.35 × 0.29 × 0.13 mm
β = 97.322 (3)°
Data collection top
Bruker SMART APEX CCD
diffractometer		18692 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2009)		14786 reflections with I > 2σ(I)
Tmin = 0.563, Tmax = 0.746Rint = 0.046
49270 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.05953 restraints
wR(F2) = 0.148H atoms treated by a mixture of independent and constrained refinement
S = 1.07Δρmax = 1.53 e Å−3
18692 reflectionsΔρmin = −0.76 e Å−3
1143 parameters
Special details top

Experimental. FT–IR bands (KBr pellet, cm-1): 1655(w), 1598(m), 1572(s), 1500(s), 1438(m), 1389(m), 1320(m), 1259(m), 1100(m), 1032(w), 927(m), 866(m), 755(m), 681(m), 651(m), 603(m), and 470(m).

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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C10.7350 (3)0.9084 (2)0.31868 (17)0.0173 (7)
C20.7214 (3)0.9888 (2)0.31474 (17)0.0182 (7)
C30.6292 (3)1.0079 (3)0.33682 (19)0.0227 (8)
H30.57840.96840.35370.027*
C40.6105 (4)1.0824 (3)0.3347 (2)0.0282 (9)
H40.54711.09390.34940.034*
C50.6855 (4)1.1403 (3)0.3108 (2)0.0342 (10)
H50.67341.19180.30920.041*
C60.7777 (4)1.1239 (3)0.2893 (2)0.0299 (9)
H60.82891.16480.27380.036*
C70.7970 (3)1.0476 (2)0.28988 (18)0.0211 (8)
C80.8083 (3)0.8217 (2)0.10425 (18)0.0165 (7)
C90.7472 (3)0.7836 (2)0.03382 (18)0.0183 (7)
C100.6736 (3)0.8210 (3)0.0078 (2)0.0237 (8)
H100.66590.87020.03600.028*
C110.6124 (4)0.7884 (3)−0.0575 (2)0.0318 (10)
H110.56240.8144−0.07380.038*
C120.6242 (4)0.7168 (3)−0.0995 (2)0.0406 (12)
H120.58320.6945−0.14480.049*
C130.6953 (4)0.6788 (3)−0.0752 (2)0.0381 (11)
H130.70270.6299−0.10400.046*
C140.7572 (3)0.7108 (3)−0.00860 (19)0.0251 (8)
C151.1539 (3)0.7569 (2)0.13292 (17)0.0166 (7)
C161.2767 (3)0.7965 (2)0.13606 (18)0.0186 (7)
C171.3110 (3)0.8163 (3)0.07890 (19)0.0233 (8)
H171.25480.80670.04040.028*
C181.4246 (4)0.8494 (3)0.0778 (2)0.0297 (9)
H181.44650.86190.03860.036*
C191.5073 (3)0.8644 (3)0.1342 (2)0.0295 (9)
H191.58580.88710.13360.035*
C201.4755 (3)0.8463 (3)0.19097 (19)0.0245 (8)
H201.53270.85710.22930.029*
C211.3603 (3)0.8121 (2)0.19326 (18)0.0185 (7)
C221.1045 (3)0.5681 (2)0.26788 (17)0.0181 (7)
C231.0764 (3)0.4758 (2)0.25878 (19)0.0210 (8)
C241.1490 (4)0.4368 (3)0.2295 (2)0.0281 (9)
H241.21150.47010.21530.034*
C251.1311 (4)0.3516 (3)0.2210 (3)0.0384 (11)
H251.18000.32590.20060.046*
C261.0410 (5)0.3038 (3)0.2427 (3)0.0454 (13)
H261.02860.24510.23750.055*
C270.9687 (4)0.3406 (3)0.2720 (3)0.0388 (11)
H270.90780.30690.28700.047*
C280.9839 (3)0.4266 (2)0.2798 (2)0.0229 (8)
C290.6962 (3)0.5839 (2)0.34485 (18)0.0170 (7)
C300.5775 (3)0.5644 (2)0.35268 (18)0.0193 (7)
C310.5095 (3)0.4788 (3)0.3384 (2)0.0281 (9)
H310.54110.43570.32430.034*
C320.3977 (4)0.4559 (3)0.3444 (3)0.0361 (10)
H320.35180.39740.33340.043*
C330.3521 (3)0.5193 (3)0.3668 (2)0.0313 (9)
H330.27510.50400.37150.038*
C340.4183 (3)0.6037 (3)0.3820 (2)0.0257 (8)
H340.38630.64610.39780.031*
C350.5311 (3)0.6289 (2)0.37494 (18)0.0204 (7)
C361.1309 (3)0.9193 (2)0.31077 (17)0.0188 (7)
C371.2511 (4)0.9685 (3)0.3086 (3)0.0376 (11)
H37A1.30470.95050.33460.056*
H37B1.26691.02960.32780.056*
H37C1.25990.95720.26190.056*
C380.7527 (3)0.5603 (2)0.17671 (18)0.0205 (8)
C390.6527 (4)0.5058 (3)0.1190 (2)0.0378 (11)
H39A0.66140.45080.10020.057*
H39B0.65030.53490.08420.057*
H39C0.58170.49630.13540.057*
C401.0971 (3)0.9664 (3)0.15302 (19)0.0240 (8)
H401.07730.90740.13090.029*
C411.0974 (4)1.0860 (3)0.2155 (2)0.0304 (9)
H411.07651.12640.24580.036*
C421.1876 (4)1.1041 (3)0.1868 (2)0.0350 (10)
H421.24161.15910.19290.042*
C431.2720 (4)1.0180 (3)0.1069 (3)0.0408 (11)
H43A1.27491.05290.07530.049*
H43B1.24860.95750.08020.049*
C441.3887 (4)1.0444 (4)0.1505 (3)0.0517 (14)
H44A1.41341.10480.17570.078*
H44B1.44271.03550.12230.078*
H44C1.38611.01000.18190.078*
C451.4080 (3)0.8109 (2)0.38991 (18)0.0209 (8)
H451.45990.82260.36140.025*
C461.2529 (4)0.7707 (3)0.42595 (19)0.0269 (9)
H461.17440.74840.42670.032*
C471.3402 (4)0.7998 (3)0.4797 (2)0.0329 (10)
H471.33470.80250.52480.040*
C481.5551 (4)0.8619 (4)0.4977 (3)0.0527 (15)
H48A1.55760.84150.53800.063*
H48B1.60700.84240.47150.063*
C491.5945 (7)0.9545 (6)0.5184 (4)0.107 (3)
H49A1.60870.97540.47950.161*
H49B1.66520.97680.55270.161*
H49C1.53620.97390.53680.161*
C501.0591 (3)0.5772 (3)0.4538 (2)0.0242 (8)
H501.07720.53080.42910.029*
C510.9833 (4)0.6726 (3)0.4804 (2)0.0315 (9)
H510.93680.70660.47750.038*
C521.0597 (4)0.6823 (3)0.5357 (2)0.0363 (10)
H521.07640.72330.57820.044*
C531.1973 (4)0.6080 (3)0.5631 (2)0.0383 (11)
H53A1.16490.58800.59930.046*
H53B1.26000.66330.58420.046*
C541.2436 (5)0.5459 (4)0.5275 (3)0.0487 (13)
H54A1.18230.49060.50780.073*
H54B1.30290.54000.55910.073*
H54C1.27640.56570.49180.073*
C550.9302 (3)0.5140 (2)0.09391 (19)0.0238 (8)
H550.96780.53530.13990.029*
C560.8500 (3)0.5057 (3)−0.00588 (19)0.0258 (9)
H560.82010.5210−0.04310.031*
C570.8496 (4)0.4272 (3)−0.00621 (19)0.0284 (9)
H570.82010.3773−0.04350.034*
C580.9067 (5)0.3603 (3)0.0823 (2)0.0461 (13)
H58A0.97420.38040.11950.055*
H58B0.91650.31640.04580.055*
C590.8014 (6)0.3212 (4)0.1065 (3)0.0619 (18)
H59A0.79330.36400.14380.093*
H59B0.80800.27280.12170.093*
H59C0.73440.30140.06980.093*
C600.9350 (3)0.8617 (3)0.44657 (19)0.0253 (8)
H600.95800.86210.40520.030*
C610.9857 (5)0.9008 (4)0.5669 (2)0.0543 (15)
H61A1.01110.95980.59540.081*
H61B1.02360.86840.58830.081*
H61C0.90300.87480.56090.081*
C621.1338 (4)0.9394 (4)0.5011 (3)0.0477 (14)
H62A1.14090.93520.45460.072*
H62B1.17960.91010.52030.072*
H62C1.16110.99960.52740.072*
C660.4691 (5)0.3119 (5)0.4271 (3)0.0678 (18)
H660.51590.35990.46330.081*
C670.2814 (6)0.2221 (4)0.3633 (4)0.079 (2)
H67A0.22770.24230.33980.119*
H67B0.23900.17500.37920.119*
H67C0.32620.20210.33250.119*
C680.3059 (6)0.3397 (5)0.4664 (3)0.0664 (18)
H68A0.36550.39160.49600.100*
H68B0.26890.30460.49340.100*
H68C0.24920.35520.44070.100*
Mn10.93174 (4)0.73894 (3)0.26039 (3)0.01331 (11)
Mn20.91283 (5)0.93489 (3)0.23478 (3)0.01607 (12)
Mn30.70262 (4)0.75746 (3)0.34634 (3)0.01606 (12)
Mn40.89055 (5)0.56145 (3)0.31923 (3)0.01619 (12)
Mn51.20451 (4)0.74267 (3)0.27382 (3)0.01525 (12)
Mn60.91421 (5)0.68460 (3)0.09187 (3)0.01735 (12)
N10.8087 (3)0.88169 (18)0.28918 (14)0.0157 (6)
N20.8782 (2)0.78744 (19)0.12949 (14)0.0155 (6)
N31.1224 (2)0.72978 (19)0.18318 (15)0.0159 (6)
N41.0339 (2)0.60427 (18)0.29254 (14)0.0154 (6)
N50.7520 (2)0.65889 (19)0.33859 (14)0.0156 (6)
N61.0400 (3)0.9991 (2)0.19402 (16)0.0207 (6)
N71.1873 (3)1.0286 (2)0.14710 (18)0.0295 (8)
N81.2962 (3)0.7787 (2)0.36986 (15)0.0185 (6)
N91.4381 (3)0.8247 (2)0.45671 (16)0.0278 (8)
N100.9831 (3)0.6061 (2)0.42876 (16)0.0215 (7)
N111.1087 (3)0.6207 (2)0.51842 (17)0.0272 (7)
N120.9013 (3)0.5605 (2)0.05783 (15)0.0193 (6)
N130.8998 (3)0.4328 (2)0.05724 (17)0.0285 (8)
N141.0143 (3)0.8996 (2)0.50281 (17)0.0298 (8)
N160.3571 (4)0.2912 (3)0.4201 (2)0.0546 (12)
O10.8154 (2)0.80558 (15)0.29986 (12)0.0158 (5)
O20.6731 (2)0.86350 (16)0.35111 (13)0.0194 (5)
O30.8877 (2)1.03649 (16)0.26824 (14)0.0224 (6)
O40.9324 (2)0.82945 (15)0.19743 (12)0.0168 (5)
O50.7943 (2)0.88760 (16)0.14020 (12)0.0195 (5)
O60.8240 (3)0.66976 (19)0.01068 (14)0.0312 (7)
O71.00397 (19)0.69177 (15)0.17379 (12)0.0158 (5)
O81.0800 (2)0.74734 (16)0.08066 (12)0.0191 (5)
O91.3382 (2)0.79776 (18)0.25096 (13)0.0221 (6)
O101.0677 (2)0.69178 (15)0.30147 (12)0.0157 (5)
O111.1935 (2)0.61166 (16)0.25236 (13)0.0205 (5)
O120.9099 (2)0.45570 (17)0.30834 (14)0.0239 (6)
O130.8652 (2)0.66919 (15)0.33249 (12)0.0153 (5)
O140.7426 (2)0.52599 (16)0.34214 (13)0.0200 (5)
O150.5925 (2)0.71167 (17)0.39152 (13)0.0218 (6)
O161.0602 (2)0.95691 (16)0.31717 (13)0.0211 (5)
O171.1059 (2)0.84037 (16)0.30492 (12)0.0181 (5)
O180.7927 (2)0.63903 (16)0.18156 (12)0.0197 (5)
O190.7904 (2)0.52364 (17)0.21420 (13)0.0247 (6)
O200.8328 (2)0.82585 (18)0.44472 (13)0.0254 (6)
O210.5729 (2)0.69487 (19)0.25284 (14)0.0281 (6)
C630.5769 (3)0.6919 (3)0.1935 (2)0.0270 (9)
H630.64580.72210.18300.032*
C640.3817 (4)0.6017 (4)0.1612 (3)0.0507 (14)
H64A0.39270.61290.21000.076*
H64B0.36070.54030.14000.076*
H64C0.32070.62110.14490.076*
C650.4863 (4)0.6460 (4)0.0750 (2)0.0481 (14)
H65A0.56200.68110.07210.072*
H65B0.42940.66920.05900.072*
H65C0.46800.58730.04710.072*
N150.4854 (3)0.6466 (3)0.14468 (18)0.0334 (9)
O220.5179 (4)0.2733 (4)0.3899 (2)0.0788 (15)
O240.5010 (5)0.2664 (4)0.2505 (3)0.0444 (19)0.67831 (1100)
H24A0.50840.25410.28690.067*0.67831 (1100)
C690.6121 (8)0.3057 (6)0.2384 (4)0.040 (2)0.67831 (1100)
H69A0.60860.34740.21410.060*0.67831 (1100)
H69B0.63610.26180.21150.060*0.67831 (1100)
H69C0.66710.33450.28130.060*0.67831 (1100)
O24B0.6205 (15)0.3611 (15)0.2170 (13)0.132 (11)0.32169 (1100)
H24B0.67220.40300.21320.198*0.32169 (1100)
C69B0.669 (2)0.3101 (19)0.244 (2)0.20 (3)0.32169 (1100)
H69D0.72830.34590.28460.300*0.32169 (1100)
H69E0.70350.28110.21140.300*0.32169 (1100)
H69F0.61030.26760.25670.300*0.32169 (1100)
O250.415 (3)0.255 (2)0.2596 (11)0.082 (17)0.12419 (1500)
H25A0.445 (3)0.294 (5)0.242 (2)0.123*0.12419 (1500)
H25B0.463 (2)0.262 (5)0.2938 (16)0.123*0.12419 (1500)
O260.1530 (10)0.8763 (16)0.9555 (9)0.051 (2)0.56763 (700)
C700.1884 (10)0.9115 (10)0.9036 (8)0.049 (3)0.56763 (700)
H70A0.14790.87010.85930.059*0.56763 (700)
H70B0.16940.96390.90660.059*0.56763 (700)
C710.3076 (10)0.9310 (14)0.9103 (12)0.069 (4)0.56763 (700)
H71A0.34750.97660.95200.103*0.56763 (700)
H71B0.33110.94990.87210.103*0.56763 (700)
H71C0.32670.88010.91150.103*0.56763 (700)
C720.0321 (9)0.8431 (7)0.9482 (6)0.052 (2)0.56763 (700)
H72A−0.00240.80680.90150.063*0.56763 (700)
H72B0.01440.80630.97820.063*0.56763 (700)
C73−0.0181 (9)0.9049 (5)0.9628 (5)0.058 (2)0.56763 (700)
H73A0.01960.94421.00760.087*0.56763 (700)
H73B−0.09910.87750.96150.087*0.56763 (700)
H73C−0.01040.93670.92940.087*0.56763 (700)
O26B0.1695 (13)0.885 (2)0.9416 (13)0.051 (2)0.43237 (700)
C70B0.2348 (15)0.9210 (14)0.8986 (10)0.049 (3)0.43237 (700)
H70C0.20620.88250.85220.059*0.43237 (700)
H70D0.22620.97630.89860.059*0.43237 (700)
C71B0.3492 (14)0.933 (2)0.9193 (17)0.069 (4)0.43237 (700)
H71D0.37180.95650.96830.103*0.43237 (700)
H71E0.39520.97320.89860.103*0.43237 (700)
H71F0.36130.87850.90570.103*0.43237 (700)
C72B0.0583 (11)0.8893 (9)0.9268 (7)0.052 (2)0.43237 (700)
H72C0.06380.94970.93560.063*0.43237 (700)
H72D0.02360.86010.87870.063*0.43237 (700)
C73B−0.0124 (11)0.8504 (11)0.9665 (7)0.058 (2)0.43237 (700)
H73D0.02290.81590.98660.087*0.43237 (700)
H73E−0.08720.81380.93810.087*0.43237 (700)
H73F−0.02180.89471.00200.087*0.43237 (700)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0182 (17)0.0149 (17)0.0152 (16)0.0064 (14)−0.0014 (13)−0.0004 (13)
C20.0204 (18)0.0166 (18)0.0139 (16)0.0087 (14)−0.0030 (13)−0.0020 (13)
C30.0247 (19)0.024 (2)0.0223 (18)0.0154 (16)0.0036 (15)0.0030 (15)
C40.031 (2)0.028 (2)0.029 (2)0.0200 (18)0.0049 (17)0.0014 (17)
C50.047 (3)0.023 (2)0.038 (2)0.024 (2)0.008 (2)0.0046 (18)
C60.039 (2)0.019 (2)0.036 (2)0.0143 (18)0.0103 (19)0.0080 (17)
C70.0227 (19)0.0170 (18)0.0185 (17)0.0089 (15)−0.0020 (14)−0.0038 (14)
C80.0114 (16)0.0150 (17)0.0234 (18)0.0050 (13)0.0032 (13)0.0061 (14)
C90.0156 (17)0.0215 (19)0.0167 (17)0.0067 (14)0.0011 (13)0.0041 (14)
C100.0214 (19)0.026 (2)0.0265 (19)0.0110 (16)0.0044 (15)0.0091 (16)
C110.028 (2)0.039 (3)0.029 (2)0.0159 (19)−0.0046 (17)0.0097 (19)
C120.040 (3)0.044 (3)0.027 (2)0.016 (2)−0.0134 (19)0.002 (2)
C130.043 (3)0.039 (3)0.025 (2)0.021 (2)−0.0104 (19)−0.0050 (19)
C140.0230 (19)0.026 (2)0.0220 (19)0.0106 (16)−0.0042 (15)0.0021 (16)
C150.0144 (16)0.0179 (18)0.0155 (16)0.0071 (14)0.0021 (13)−0.0002 (13)
C160.0157 (17)0.0179 (18)0.0187 (17)0.0051 (14)0.0013 (14)0.0012 (14)
C170.0223 (19)0.027 (2)0.0175 (17)0.0078 (16)0.0030 (15)0.0022 (15)
C180.027 (2)0.036 (2)0.023 (2)0.0057 (18)0.0106 (17)0.0071 (17)
C190.0163 (18)0.040 (3)0.028 (2)0.0062 (17)0.0068 (16)0.0042 (18)
C200.0149 (17)0.030 (2)0.0221 (19)0.0047 (16)0.0011 (14)0.0020 (16)
C210.0157 (17)0.0207 (18)0.0164 (16)0.0052 (14)0.0030 (13)0.0022 (14)
C220.0184 (17)0.0192 (18)0.0151 (16)0.0094 (15)−0.0009 (13)0.0006 (14)
C230.0231 (19)0.0188 (19)0.0224 (18)0.0135 (15)0.0024 (15)0.0015 (15)
C240.029 (2)0.028 (2)0.030 (2)0.0166 (18)0.0070 (17)0.0021 (17)
C250.039 (3)0.028 (2)0.055 (3)0.024 (2)0.016 (2)0.006 (2)
C260.051 (3)0.022 (2)0.073 (4)0.023 (2)0.025 (3)0.010 (2)
C270.045 (3)0.022 (2)0.059 (3)0.018 (2)0.022 (2)0.015 (2)
C280.0240 (19)0.0186 (19)0.029 (2)0.0135 (16)0.0047 (16)0.0041 (15)
C290.0152 (17)0.0174 (17)0.0190 (17)0.0075 (14)0.0041 (13)0.0036 (14)
C300.0123 (16)0.0206 (19)0.0234 (18)0.0046 (14)0.0025 (14)0.0054 (15)
C310.021 (2)0.023 (2)0.038 (2)0.0069 (16)0.0048 (17)0.0066 (17)
C320.022 (2)0.028 (2)0.053 (3)0.0008 (18)0.008 (2)0.012 (2)
C330.0144 (18)0.037 (2)0.039 (2)0.0051 (17)0.0059 (17)0.0095 (19)
C340.0153 (18)0.031 (2)0.030 (2)0.0090 (16)0.0041 (15)0.0079 (17)
C350.0208 (18)0.0218 (19)0.0184 (17)0.0083 (15)0.0040 (14)0.0042 (14)
C360.0199 (18)0.0170 (18)0.0153 (16)0.0050 (14)−0.0016 (13)0.0020 (14)
C370.025 (2)0.023 (2)0.061 (3)0.0047 (18)0.006 (2)0.012 (2)
C380.0169 (17)0.023 (2)0.0206 (18)0.0082 (15)0.0053 (14)0.0016 (15)
C390.027 (2)0.029 (2)0.041 (3)0.0025 (19)−0.0087 (19)−0.002 (2)
C400.029 (2)0.0207 (19)0.0220 (18)0.0083 (16)0.0065 (16)0.0047 (15)
C410.034 (2)0.018 (2)0.036 (2)0.0083 (17)0.0074 (19)0.0034 (17)
C420.036 (2)0.020 (2)0.045 (3)0.0047 (18)0.011 (2)0.0068 (19)
C430.045 (3)0.035 (3)0.044 (3)0.010 (2)0.026 (2)0.011 (2)
C440.036 (3)0.044 (3)0.073 (4)0.011 (2)0.021 (3)0.010 (3)
C450.0188 (18)0.0205 (19)0.0202 (18)0.0089 (15)−0.0005 (14)−0.0003 (14)
C460.026 (2)0.033 (2)0.0175 (18)0.0077 (17)0.0063 (15)0.0018 (16)
C470.035 (2)0.042 (3)0.0166 (19)0.014 (2)0.0026 (17)−0.0013 (17)
C480.031 (2)0.075 (4)0.033 (2)0.024 (3)−0.013 (2)−0.018 (2)
C490.081 (5)0.116 (6)0.075 (5)−0.028 (4)0.001 (4)0.024 (5)
C500.0230 (19)0.026 (2)0.0247 (19)0.0081 (16)0.0063 (16)0.0083 (16)
C510.037 (2)0.033 (2)0.027 (2)0.017 (2)0.0089 (18)0.0061 (18)
C520.048 (3)0.034 (2)0.024 (2)0.016 (2)0.0058 (19)0.0020 (18)
C530.031 (2)0.054 (3)0.031 (2)0.014 (2)−0.0006 (19)0.018 (2)
C540.043 (3)0.071 (4)0.044 (3)0.028 (3)0.010 (2)0.026 (3)
C550.026 (2)0.021 (2)0.0176 (17)0.0087 (16)−0.0018 (15)−0.0051 (15)
C560.023 (2)0.027 (2)0.0199 (18)0.0122 (17)−0.0036 (15)−0.0068 (16)
C570.032 (2)0.026 (2)0.0183 (18)0.0135 (18)−0.0049 (16)−0.0082 (16)
C580.074 (4)0.027 (2)0.033 (2)0.028 (3)−0.008 (2)−0.002 (2)
C590.112 (6)0.031 (3)0.044 (3)0.022 (3)0.023 (3)0.013 (2)
C600.027 (2)0.025 (2)0.0193 (18)0.0109 (17)0.0016 (15)−0.0045 (15)
C610.048 (3)0.074 (4)0.024 (2)0.014 (3)0.001 (2)−0.002 (2)
C620.027 (2)0.052 (3)0.042 (3)0.009 (2)−0.007 (2)−0.014 (2)
C660.050 (4)0.092 (5)0.051 (4)0.020 (4)0.001 (3)0.011 (3)
C670.059 (4)0.061 (4)0.094 (6)0.013 (3)0.006 (4)−0.004 (4)
C680.076 (4)0.086 (5)0.047 (3)0.043 (4)0.018 (3)0.017 (3)
Mn10.0120 (2)0.0129 (3)0.0137 (2)0.0055 (2)0.00118 (19)0.00076 (19)
Mn20.0186 (3)0.0123 (3)0.0167 (3)0.0070 (2)0.0027 (2)0.0014 (2)
Mn30.0145 (3)0.0161 (3)0.0194 (3)0.0084 (2)0.0055 (2)0.0035 (2)
Mn40.0160 (3)0.0133 (3)0.0207 (3)0.0072 (2)0.0051 (2)0.0043 (2)
Mn50.0103 (2)0.0181 (3)0.0145 (2)0.0044 (2)−0.00008 (19)0.0016 (2)
Mn60.0154 (3)0.0165 (3)0.0144 (3)0.0073 (2)−0.0043 (2)−0.0044 (2)
N10.0192 (15)0.0108 (14)0.0165 (14)0.0069 (12)0.0010 (11)0.0022 (11)
N20.0164 (14)0.0156 (15)0.0111 (13)0.0055 (12)−0.0007 (11)−0.0007 (11)
N30.0085 (13)0.0148 (15)0.0190 (14)0.0021 (11)−0.0012 (11)−0.0007 (12)
N40.0141 (14)0.0126 (14)0.0181 (14)0.0044 (11)0.0024 (11)0.0026 (11)
N50.0103 (13)0.0183 (15)0.0180 (14)0.0062 (11)0.0035 (11)0.0031 (12)
N60.0212 (16)0.0165 (16)0.0219 (15)0.0058 (13)0.0023 (13)0.0033 (12)
N70.0310 (19)0.0230 (18)0.0323 (19)0.0048 (15)0.0117 (15)0.0072 (15)
N80.0165 (15)0.0201 (16)0.0178 (14)0.0080 (12)0.0013 (12)0.0026 (12)
N90.0269 (18)0.0290 (19)0.0208 (16)0.0152 (15)−0.0064 (14)−0.0067 (14)
N100.0206 (16)0.0218 (17)0.0214 (16)0.0067 (13)0.0046 (13)0.0059 (13)
N110.0237 (17)0.036 (2)0.0219 (16)0.0079 (15)0.0031 (14)0.0119 (15)
N120.0176 (15)0.0177 (16)0.0157 (14)0.0066 (12)−0.0029 (12)−0.0051 (12)
N130.037 (2)0.0232 (18)0.0223 (16)0.0166 (15)−0.0021 (14)−0.0030 (14)
N140.0277 (18)0.032 (2)0.0218 (17)0.0106 (15)−0.0009 (14)−0.0048 (14)
N160.051 (3)0.056 (3)0.052 (3)0.016 (2)0.010 (2)0.009 (2)
O10.0162 (12)0.0136 (12)0.0199 (12)0.0084 (10)0.0040 (10)0.0046 (10)
O20.0184 (12)0.0194 (13)0.0232 (13)0.0106 (11)0.0065 (10)0.0047 (11)
O30.0235 (14)0.0144 (13)0.0294 (14)0.0086 (11)0.0064 (11)0.0039 (11)
O40.0211 (13)0.0142 (12)0.0123 (11)0.0073 (10)0.0009 (10)−0.0013 (9)
O50.0188 (13)0.0204 (13)0.0200 (12)0.0098 (11)0.0024 (10)0.0042 (10)
O60.0363 (16)0.0292 (16)0.0212 (14)0.0203 (13)−0.0119 (12)−0.0075 (12)
O70.0105 (11)0.0173 (13)0.0158 (12)0.0049 (10)−0.0006 (9)−0.0009 (10)
O80.0169 (12)0.0233 (14)0.0128 (11)0.0063 (10)−0.0005 (9)0.0000 (10)
O90.0120 (12)0.0314 (15)0.0177 (12)0.0032 (11)−0.0003 (10)0.0052 (11)
O100.0147 (12)0.0127 (12)0.0180 (12)0.0052 (10)0.0024 (9)0.0012 (9)
O110.0159 (12)0.0208 (14)0.0256 (13)0.0091 (11)0.0059 (10)0.0035 (11)
O120.0297 (15)0.0174 (13)0.0303 (15)0.0136 (11)0.0117 (12)0.0077 (11)
O130.0121 (11)0.0165 (12)0.0175 (12)0.0067 (10)0.0032 (9)0.0030 (10)
O140.0185 (13)0.0169 (13)0.0262 (13)0.0071 (10)0.0070 (11)0.0067 (11)
O150.0194 (13)0.0233 (14)0.0262 (14)0.0101 (11)0.0110 (11)0.0069 (11)
O160.0232 (13)0.0187 (13)0.0192 (13)0.0097 (11)−0.0002 (10)0.0004 (10)
O170.0158 (12)0.0167 (13)0.0195 (12)0.0061 (10)0.0010 (10)0.0020 (10)
O180.0154 (12)0.0210 (14)0.0190 (12)0.0063 (10)0.0009 (10)0.0003 (10)
O190.0287 (15)0.0189 (14)0.0239 (14)0.0083 (12)0.0035 (11)0.0025 (11)
O200.0238 (14)0.0272 (15)0.0206 (13)0.0086 (12)0.0016 (11)0.0004 (11)
O210.0215 (14)0.0301 (16)0.0295 (15)0.0100 (12)0.0004 (12)0.0039 (12)
C630.0184 (19)0.027 (2)0.031 (2)0.0115 (16)−0.0032 (16)0.0000 (17)
C640.036 (3)0.081 (4)0.033 (3)0.020 (3)0.008 (2)0.013 (3)
C650.029 (2)0.069 (4)0.030 (2)0.010 (2)0.002 (2)−0.003 (2)
N150.0189 (17)0.045 (2)0.0253 (18)0.0117 (16)−0.0036 (14)−0.0079 (16)
O220.063 (3)0.118 (4)0.058 (3)0.044 (3)0.015 (2)0.014 (3)
O240.049 (4)0.044 (3)0.034 (3)0.015 (3)0.000 (2)0.007 (2)
C690.041 (5)0.043 (5)0.047 (4)0.024 (4)0.012 (4)0.022 (4)
O24B0.059 (11)0.108 (18)0.16 (2)−0.008 (11)0.026 (13)−0.034 (17)
C69B0.060 (19)0.065 (19)0.51 (10)0.025 (16)0.08 (3)0.15 (4)
O250.06 (3)0.06 (2)0.08 (3)−0.009 (17)0.03 (2)−0.020 (18)
O260.048 (4)0.066 (6)0.040 (8)0.020 (5)0.023 (3)0.010 (5)
C700.034 (8)0.054 (5)0.061 (5)0.017 (7)0.013 (7)0.016 (4)
C710.025 (10)0.054 (5)0.131 (10)0.009 (9)0.024 (11)0.034 (6)
C720.066 (6)0.058 (5)0.063 (5)0.038 (5)0.034 (4)0.040 (4)
C730.064 (5)0.078 (7)0.047 (5)0.039 (6)0.010 (4)0.027 (5)
O26B0.048 (4)0.066 (6)0.040 (8)0.020 (5)0.023 (3)0.010 (5)
C70B0.034 (8)0.054 (5)0.061 (5)0.017 (7)0.013 (7)0.016 (4)
C71B0.025 (10)0.054 (5)0.131 (10)0.009 (9)0.024 (11)0.034 (6)
C72B0.066 (6)0.058 (5)0.063 (5)0.038 (5)0.034 (4)0.040 (4)
C73B0.064 (5)0.078 (7)0.047 (5)0.039 (6)0.010 (4)0.027 (5)
Geometric parameters (Å, º) top
C1—O21.298 (4)C56—C571.347 (6)
C1—N11.316 (4)C56—N121.383 (4)
C1—C21.462 (5)C56—H560.9500
C2—C31.403 (5)C57—N131.368 (5)
C2—C71.410 (6)C57—H570.9500
C3—C41.382 (5)C58—N131.483 (6)
C3—H30.9500C58—C591.504 (8)
C4—C51.386 (7)C58—H58A0.9900
C4—H40.9500C58—H58B0.9900
C5—C61.380 (6)C59—H59A0.9800
C5—H50.9500C59—H59B0.9800
C6—C71.408 (5)C59—H59C0.9800
C6—H60.9500C60—O201.240 (5)
C7—O31.332 (4)C60—N141.327 (5)
C8—O51.279 (4)C60—H600.9500
C8—N21.322 (4)C61—N141.434 (6)
C8—C91.469 (5)C61—H61A0.9800
C9—C101.404 (5)C61—H61B0.9800
C9—C141.406 (5)C61—H61C0.9800
C10—C111.376 (6)C62—N141.462 (6)
C10—H100.9500C62—H62A0.9800
C11—C121.397 (6)C62—H62B0.9800
C11—H110.9500C62—H62C0.9800
C12—C131.374 (6)C66—O221.247 (8)
C12—H120.9500C66—N161.326 (8)
C13—C141.402 (5)C66—H660.9500
C13—H130.9500C67—N161.449 (8)
C14—O61.333 (5)C67—H67A0.9800
C15—O81.288 (4)C67—H67B0.9800
C15—N31.309 (5)C67—H67C0.9800
C15—C161.476 (5)C68—N161.471 (7)
C16—C171.406 (5)C68—H68A0.9800
C16—C211.407 (5)C68—H68B0.9800
C17—C181.377 (6)C68—H68C0.9800
C17—H170.9500Mn1—O182.205 (3)
C18—C191.390 (6)Mn1—O72.229 (2)
C18—H180.9500Mn1—O132.235 (2)
C19—C201.378 (6)Mn1—O12.243 (2)
C19—H190.9500Mn1—O172.263 (3)
C20—C211.403 (5)Mn1—O42.264 (3)
C20—H200.9500Mn1—O102.265 (2)
C21—O91.338 (4)Mn2—O31.860 (3)
C22—O111.275 (5)Mn2—O41.901 (2)
C22—N41.322 (4)Mn2—N12.001 (3)
C22—C231.476 (5)Mn2—N62.059 (3)
C23—C281.405 (6)Mn2—O52.141 (3)
C23—C241.408 (5)Mn2—O162.243 (3)
C24—C251.377 (6)Mn3—O151.862 (3)
C24—H240.9500Mn3—O11.917 (3)
C25—C261.382 (7)Mn3—O21.951 (3)
C25—H250.9500Mn3—N51.955 (3)
C26—C271.385 (6)Mn3—O212.192 (3)
C26—H260.9500Mn3—O202.273 (3)
C27—C281.399 (6)Mn4—O121.872 (3)
C27—H270.9500Mn4—O131.936 (2)
C28—O121.329 (4)Mn4—O141.938 (3)
C29—O141.293 (4)Mn4—N41.941 (3)
C29—N51.314 (5)Mn4—O192.235 (3)
C29—C301.470 (5)Mn4—N102.276 (3)
C30—C311.397 (5)Mn5—O91.849 (3)
C30—C351.417 (5)Mn5—O101.912 (2)
C31—C321.375 (6)Mn5—N31.975 (3)
C31—H310.9500Mn5—N82.042 (3)
C32—C331.395 (6)Mn5—O112.148 (3)
C32—H320.9500Mn5—O172.398 (2)
C33—C341.372 (6)Mn6—O61.841 (3)
C33—H330.9500Mn6—O71.890 (2)
C34—C351.394 (5)Mn6—N21.969 (3)
C34—H340.9500Mn6—N122.032 (3)
C35—O151.332 (5)Mn6—O82.112 (3)
C36—O161.253 (4)N1—O11.403 (4)
C36—O171.267 (4)N2—O41.411 (3)
C36—C371.507 (6)N3—O71.403 (4)
C37—H37A0.9800N4—O101.392 (4)
C37—H37B0.9800N5—O131.409 (3)
C37—H37C0.9800O21—C631.242 (5)
C38—O191.250 (5)C63—N151.328 (5)
C38—O181.266 (5)C63—H630.9500
C38—C391.515 (5)C64—N151.433 (6)
C39—H39A0.9800C64—H64A0.9800
C39—H39B0.9800C64—H64B0.9800
C39—H39C0.9800C64—H64C0.9800
C40—N61.324 (5)C65—N151.463 (6)
C40—N71.346 (5)C65—H65A0.9800
C40—H400.9500C65—H65B0.9800
C41—C421.342 (6)C65—H65C0.9800
C41—N61.380 (5)O24—C691.442 (11)
C41—H410.9500O24—H24A0.8400
C42—N71.367 (5)O24—H25A0.98 (7)
C42—H420.9500O24—H25B1.09 (3)
C43—N71.471 (6)C69—H69A0.9800
C43—C441.505 (7)C69—H69B0.9800
C43—H43A0.9900C69—H69C0.9800
C43—H43B0.9900O24B—C69B1.40 (2)
C44—H44A0.9800O24B—H24B0.8400
C44—H44B0.9800C69B—H69D0.9800
C44—H44C0.9800C69B—H69E0.9800
C45—N81.317 (5)C69B—H69F0.9800
C45—N91.349 (5)O25—H25A0.84 (2)
C45—H450.9500O25—H25A0.84 (2)
C46—C471.349 (6)O25—H25B0.835 (18)
C46—N81.377 (5)O26—C701.423 (11)
C46—H460.9500O26—C721.429 (13)
C47—N91.366 (6)C70—C711.417 (11)
C47—H470.9500C70—H70A0.9900
C48—C491.453 (10)C70—H70B0.9900
C48—N91.473 (5)C71—H71A0.9800
C48—H48A0.9900C71—H71B0.9800
C48—H48B0.9900C71—H71C0.9800
C49—H49A0.9800C72—C731.388 (10)
C49—H49B0.9800C72—H72A0.9900
C49—H49C0.9800C72—H72B0.9900
C50—N101.313 (5)C73—H73A0.9800
C50—N111.347 (5)C73—H73B0.9800
C50—H500.9500C73—H73C0.9800
C51—C521.355 (6)O26B—C70B1.421 (14)
C51—N101.377 (5)O26B—C72B1.424 (13)
C51—H510.9500C70B—C71B1.387 (13)
C52—N111.381 (6)C70B—H70C0.9900
C52—H520.9500C70B—H70D0.9900
C53—N111.467 (5)C71B—H71D0.9800
C53—C541.467 (7)C71B—H71E0.9800
C53—H53A0.9900C71B—H71F0.9800
C53—H53B0.9900C72B—C73B1.422 (11)
C54—H54A0.9800C72B—H72C0.9900
C54—H54B0.9800C72B—H72D0.9900
C54—H54C0.9800C73B—H73D0.9800
C55—N121.318 (5)C73B—H73E0.9800
C55—N131.335 (5)C73B—H73F0.9800
C55—H550.9500
O2—C1—N1120.4 (3)O18—Mn1—O1387.02 (10)
O2—C1—C2119.4 (3)O7—Mn1—O13127.19 (9)
N1—C1—C2120.2 (3)O18—Mn1—O193.10 (9)
C3—C2—C7119.0 (3)O7—Mn1—O1147.92 (9)
C3—C2—C1118.3 (3)O13—Mn1—O177.71 (9)
C7—C2—C1122.7 (3)O18—Mn1—O17157.00 (9)
C4—C3—C2121.8 (4)O7—Mn1—O1786.99 (9)
C4—C3—H3119.1O13—Mn1—O17112.73 (9)
C2—C3—H3119.1O1—Mn1—O17102.30 (9)
C3—C4—C5119.0 (4)O18—Mn1—O488.74 (9)
C3—C4—H4120.5O7—Mn1—O475.21 (9)
C5—C4—H4120.5O13—Mn1—O4153.77 (9)
C6—C5—C4120.7 (4)O1—Mn1—O476.70 (9)
C6—C5—H5119.7O17—Mn1—O478.48 (9)
C4—C5—H5119.7O18—Mn1—O10113.49 (9)
C5—C6—C7121.1 (4)O7—Mn1—O1073.78 (9)
C5—C6—H6119.4O13—Mn1—O1072.20 (9)
C7—C6—H6119.4O1—Mn1—O10138.01 (9)
O3—C7—C6117.4 (4)O17—Mn1—O1064.99 (9)
O3—C7—C2124.1 (3)O4—Mn1—O10132.60 (9)
C6—C7—C2118.4 (4)O3—Mn2—O4177.37 (11)
O5—C8—N2120.8 (3)O3—Mn2—N188.86 (12)
O5—C8—C9120.1 (3)O4—Mn2—N190.97 (11)
N2—C8—C9119.1 (3)O3—Mn2—N689.00 (12)
C10—C9—C14118.3 (3)O4—Mn2—N691.59 (12)
C10—C9—C8118.3 (3)N1—Mn2—N6170.25 (12)
C14—C9—C8123.4 (3)O3—Mn2—O599.06 (11)
C11—C10—C9121.7 (4)O4—Mn2—O578.37 (10)
C11—C10—H10119.1N1—Mn2—O598.38 (11)
C9—C10—H10119.1N6—Mn2—O591.35 (11)
C10—C11—C12119.6 (4)O3—Mn2—O1697.26 (11)
C10—C11—H11120.2O4—Mn2—O1685.36 (10)
C12—C11—H11120.2N1—Mn2—O1688.14 (11)
C13—C12—C11119.8 (4)N6—Mn2—O1682.69 (11)
C13—C12—H12120.1O5—Mn2—O16162.52 (9)
C11—C12—H12120.1O15—Mn3—O1179.39 (11)
C12—C13—C14121.2 (4)O15—Mn3—O297.41 (11)
C12—C13—H13119.4O1—Mn3—O281.99 (10)
C14—C13—H13119.4O15—Mn3—N590.10 (12)
O6—C14—C13117.1 (4)O1—Mn3—N590.51 (11)
O6—C14—C9123.5 (3)O2—Mn3—N5172.17 (12)
C13—C14—C9119.4 (4)O15—Mn3—O2188.05 (12)
O8—C15—N3121.1 (3)O1—Mn3—O2191.88 (11)
O8—C15—C16120.2 (3)O2—Mn3—O2189.67 (11)
N3—C15—C16118.6 (3)N5—Mn3—O2192.83 (11)
C17—C16—C21119.1 (3)O15—Mn3—O2090.96 (11)
C17—C16—C15118.6 (3)O1—Mn3—O2089.09 (10)
C21—C16—C15122.3 (3)O2—Mn3—O2088.31 (11)
C18—C17—C16121.1 (4)N5—Mn3—O2089.34 (11)
C18—C17—H17119.4O21—Mn3—O20177.61 (10)
C16—C17—H17119.4O12—Mn4—O13177.47 (11)
C17—C18—C19119.7 (4)O12—Mn4—O1495.31 (11)
C17—C18—H18120.1O13—Mn4—O1482.24 (10)
C19—C18—H18120.1O12—Mn4—N489.32 (12)
C20—C19—C18120.1 (4)O13—Mn4—N493.16 (11)
C20—C19—H19120.0O14—Mn4—N4174.60 (12)
C18—C19—H19120.0O12—Mn4—O1992.92 (11)
C19—C20—C21121.3 (4)O13—Mn4—O1987.52 (10)
C19—C20—H20119.3O14—Mn4—O1984.70 (11)
C21—C20—H20119.3N4—Mn4—O1992.31 (11)
O9—C21—C20116.8 (3)O12—Mn4—N1090.88 (12)
O9—C21—C16124.6 (3)O13—Mn4—N1088.56 (11)
C20—C21—C16118.6 (3)O14—Mn4—N1092.21 (11)
O11—C22—N4120.9 (3)N4—Mn4—N1090.50 (12)
O11—C22—C23121.3 (3)O19—Mn4—N10175.30 (11)
N4—C22—C23117.8 (3)O9—Mn5—O10176.63 (11)
C28—C23—C24119.4 (4)O9—Mn5—N388.23 (12)
C28—C23—C22123.1 (3)O10—Mn5—N393.31 (11)
C24—C23—C22117.5 (4)O9—Mn5—N887.30 (12)
C25—C24—C23121.3 (4)O10—Mn5—N890.69 (11)
C25—C24—H24119.3N3—Mn5—N8169.82 (13)
C23—C24—H24119.3O9—Mn5—O11104.93 (11)
C24—C25—C26119.2 (4)O10—Mn5—O1177.94 (10)
C24—C25—H25120.4N3—Mn5—O1194.58 (11)
C26—C25—H25120.4N8—Mn5—O1195.41 (11)
C25—C26—C27120.7 (4)O9—Mn5—O17109.67 (11)
C25—C26—H26119.6O10—Mn5—O1767.64 (9)
C27—C26—H26119.6N3—Mn5—O1781.70 (10)
C26—C27—C28121.0 (4)N8—Mn5—O1791.20 (10)
C26—C27—H27119.5O11—Mn5—O17145.02 (9)
C28—C27—H27119.5O6—Mn6—O7176.15 (12)
O12—C28—C27116.3 (4)O6—Mn6—N289.00 (12)
O12—C28—C23125.2 (3)O7—Mn6—N294.26 (11)
C27—C28—C23118.4 (4)O6—Mn6—N1287.48 (12)
O14—C29—N5121.2 (3)O7—Mn6—N1288.78 (11)
O14—C29—C30119.4 (3)N2—Mn6—N12161.73 (13)
N5—C29—C30119.4 (3)O6—Mn6—O8103.09 (13)
C31—C30—C35119.5 (3)O7—Mn6—O878.56 (10)
C31—C30—C29118.0 (3)N2—Mn6—O897.25 (11)
C35—C30—C29122.5 (3)N12—Mn6—O8101.01 (11)
C32—C31—C30121.2 (4)C1—N1—O1113.5 (3)
C32—C31—H31119.4C1—N1—Mn2129.7 (2)
C30—C31—H31119.4O1—N1—Mn2116.9 (2)
C31—C32—C33119.4 (4)C8—N2—O4114.1 (3)
C31—C32—H32120.3C8—N2—Mn6132.1 (2)
C33—C32—H32120.3O4—N2—Mn6113.7 (2)
C34—C33—C32120.1 (4)C15—N3—O7113.4 (3)
C34—C33—H33119.9C15—N3—Mn5133.4 (2)
C32—C33—H33119.9O7—N3—Mn5112.7 (2)
C33—C34—C35121.8 (4)C22—N4—O10114.5 (3)
C33—C34—H34119.1C22—N4—Mn4133.7 (3)
C35—C34—H34119.1O10—N4—Mn4111.80 (19)
O15—C35—C34119.5 (3)C29—N5—O13113.3 (3)
O15—C35—C30122.5 (3)C29—N5—Mn3128.1 (2)
C34—C35—C30118.0 (4)O13—N5—Mn3118.2 (2)
O16—C36—O17123.0 (3)C40—N6—C41106.3 (3)
O16—C36—C37119.5 (3)C40—N6—Mn2127.7 (3)
O17—C36—C37117.6 (3)C41—N6—Mn2124.8 (3)
C36—C37—H37A109.5C40—N7—C42107.4 (4)
C36—C37—H37B109.5C40—N7—C43126.8 (4)
H37A—C37—H37B109.5C42—N7—C43125.8 (4)
C36—C37—H37C109.5C45—N8—C46106.7 (3)
H37A—C37—H37C109.5C45—N8—Mn5126.9 (3)
H37B—C37—H37C109.5C46—N8—Mn5126.4 (3)
O19—C38—O18125.7 (3)C45—N9—C47107.5 (3)
O19—C38—C39117.4 (4)C45—N9—C48126.3 (4)
O18—C38—C39116.8 (3)C47—N9—C48126.2 (4)
C38—C39—H39A109.5C50—N10—C51105.2 (3)
C38—C39—H39B109.5C50—N10—Mn4124.9 (3)
H39A—C39—H39B109.5C51—N10—Mn4129.4 (3)
C38—C39—H39C109.5C50—N11—C52106.1 (3)
H39A—C39—H39C109.5C50—N11—C53128.6 (4)
H39B—C39—H39C109.5C52—N11—C53125.3 (4)
N6—C40—N7110.4 (3)C55—N12—C56106.2 (3)
N6—C40—H40124.8C55—N12—Mn6126.6 (2)
N7—C40—H40124.8C56—N12—Mn6127.0 (3)
C42—C41—N6108.9 (4)C55—N13—C57107.3 (3)
C42—C41—H41125.5C55—N13—C58126.4 (4)
N6—C41—H41125.5C57—N13—C58126.0 (3)
C41—C42—N7107.1 (4)C60—N14—C61121.0 (4)
C41—C42—H42126.5C60—N14—C62121.0 (4)
N7—C42—H42126.5C61—N14—C62118.1 (4)
N7—C43—C44111.6 (4)C66—N16—C67120.0 (6)
N7—C43—H43A109.3C66—N16—C68121.9 (6)
C44—C43—H43A109.3C67—N16—C68118.0 (5)
N7—C43—H43B109.3N1—O1—Mn3112.10 (19)
C44—C43—H43B109.3N1—O1—Mn1125.31 (19)
H43A—C43—H43B108.0Mn3—O1—Mn1122.37 (12)
C43—C44—H44A109.5C1—O2—Mn3111.7 (2)
C43—C44—H44B109.5C7—O3—Mn2128.4 (2)
H44A—C44—H44B109.5N2—O4—Mn2115.97 (19)
C43—C44—H44C109.5N2—O4—Mn1113.29 (18)
H44A—C44—H44C109.5Mn2—O4—Mn1119.61 (11)
H44B—C44—H44C109.5C8—O5—Mn2109.5 (2)
N8—C45—N9110.2 (3)C14—O6—Mn6132.6 (2)
N8—C45—H45124.9N3—O7—Mn6117.0 (2)
N9—C45—H45124.9N3—O7—Mn1114.51 (18)
C47—C46—N8108.8 (4)Mn6—O7—Mn1111.00 (11)
C47—C46—H46125.6C15—O8—Mn6109.9 (2)
N8—C46—H46125.6C21—O9—Mn5131.9 (2)
C46—C47—N9106.8 (4)N4—O10—Mn5116.74 (19)
C46—C47—H47126.6N4—O10—Mn1115.60 (18)
N9—C47—H47126.6Mn5—O10—Mn1108.37 (11)
C49—C48—N9111.8 (5)C22—O11—Mn5109.9 (2)
C49—C48—H48A109.3C28—O12—Mn4129.7 (3)
N9—C48—H48A109.3N5—O13—Mn4110.59 (19)
C49—C48—H48B109.3N5—O13—Mn1116.94 (18)
N9—C48—H48B109.3Mn4—O13—Mn1112.59 (11)
H48A—C48—H48B107.9C29—O14—Mn4111.3 (2)
C48—C49—H49A109.5C35—O15—Mn3123.3 (2)
C48—C49—H49B109.5C36—O16—Mn2123.5 (2)
H49A—C49—H49B109.5C36—O17—Mn1125.9 (2)
C48—C49—H49C109.5C36—O17—Mn5132.5 (2)
H49A—C49—H49C109.5Mn1—O17—Mn593.39 (9)
H49B—C49—H49C109.5C38—O18—Mn1127.5 (2)
N10—C50—N11112.5 (4)C38—O19—Mn4136.3 (2)
N10—C50—H50123.8C60—O20—Mn3122.1 (2)
N11—C50—H50123.8C63—O21—Mn3132.1 (3)
C52—C51—N10109.7 (4)O21—C63—N15120.5 (4)
C52—C51—H51125.1O21—C63—H63119.8
N10—C51—H51125.1N15—C63—H63119.8
C51—C52—N11106.5 (4)N15—C64—H64A109.5
C51—C52—H52126.8N15—C64—H64B109.5
N11—C52—H52126.8H64A—C64—H64B109.5
N11—C53—C54112.3 (4)N15—C64—H64C109.5
N11—C53—H53A109.2H64A—C64—H64C109.5
C54—C53—H53A109.2H64B—C64—H64C109.5
N11—C53—H53B109.2N15—C65—H65A109.5
C54—C53—H53B109.2N15—C65—H65B109.5
H53A—C53—H53B107.9H65A—C65—H65B109.5
C53—C54—H54A109.5N15—C65—H65C109.5
C53—C54—H54B109.5H65A—C65—H65C109.5
H54A—C54—H54B109.5H65B—C65—H65C109.5
C53—C54—H54C109.5C63—N15—C64119.3 (4)
H54A—C54—H54C109.5C63—N15—C65121.4 (4)
H54B—C54—H54C109.5C64—N15—C65119.2 (4)
N12—C55—N13111.0 (3)C69—O24—H25A115.7 (18)
N12—C55—H55124.5H24A—O24—H25A117.5
N13—C55—H55124.5C69—O24—H25B137.2 (19)
C57—C56—N12108.5 (4)H25A—O24—H25B81 (4)
C57—C56—H56125.8C69B—O24B—H24B109.5
N12—C56—H56125.8O24B—C69B—H69D109.5
C56—C57—N13107.0 (3)O24B—C69B—H69E109.5
C56—C57—H57126.5H69D—C69B—H69E109.5
N13—C57—H57126.5O24B—C69B—H69F109.5
N13—C58—C59111.5 (4)H69D—C69B—H69F109.5
N13—C58—H58A109.3H69E—C69B—H69F109.5
C59—C58—H58A109.3H25A—O25—H25B107 (3)
N13—C58—H58B109.3H25A—O25—H25B107 (3)
C59—C58—H58B109.3C70—O26—C72114.0 (10)
H58A—C58—H58B108.0C71—C70—O26109.2 (10)
C58—C59—H59A109.5C71—C70—H70A109.8
C58—C59—H59B109.5O26—C70—H70A109.8
H59A—C59—H59B109.5C71—C70—H70B109.8
C58—C59—H59C109.5O26—C70—H70B109.8
H59A—C59—H59C109.5H70A—C70—H70B108.3
H59B—C59—H59C109.5C73—C72—O26114.4 (12)
O20—C60—N14123.9 (4)C73—C72—H72A108.7
O20—C60—H60118.0O26—C72—H72A108.7
N14—C60—H60118.0C73—C72—H72B108.7
N14—C61—H61A109.5O26—C72—H72B108.7
N14—C61—H61B109.5H72A—C72—H72B107.6
H61A—C61—H61B109.5C70B—O26B—C72B108.9 (14)
N14—C61—H61C109.5C71B—C70B—O26B110.9 (13)
H61A—C61—H61C109.5C71B—C70B—H70C109.5
H61B—C61—H61C109.5O26B—C70B—H70C109.5
N14—C62—H62A109.5C71B—C70B—H70D109.5
N14—C62—H62B109.5O26B—C70B—H70D109.5
H62A—C62—H62B109.5H70C—C70B—H70D108.0
N14—C62—H62C109.5C70B—C71B—H71D109.5
H62A—C62—H62C109.5C70B—C71B—H71E109.5
H62B—C62—H62C109.5H71D—C71B—H71E109.5
O22—C66—N16125.2 (7)C70B—C71B—H71F109.5
O22—C66—H66117.4H71D—C71B—H71F109.5
N16—C66—H66117.4H71E—C71B—H71F109.5
N16—C67—H67A109.5C73B—C72B—O26B111.0 (11)
N16—C67—H67B109.5C73B—C72B—H72C109.4
H67A—C67—H67B109.5O26B—C72B—H72C109.4
N16—C67—H67C109.5C73B—C72B—H72D109.4
H67A—C67—H67C109.5O26B—C72B—H72D109.4
H67B—C67—H67C109.5H72C—C72B—H72D108.0
N16—C68—H68A109.5C72B—C73B—H73D109.5
N16—C68—H68B109.5C72B—C73B—H73E109.5
H68A—C68—H68B109.5H73D—C73B—H73E109.5
N16—C68—H68C109.5C72B—C73B—H73F109.5
H68A—C68—H68C109.5H73D—C73B—H73F109.5
H68B—C68—H68C109.5H73E—C73B—H73F109.5
O18—Mn1—O771.17 (9)
O2—C1—C2—C3−10.1 (5)O18—Mn1—O1—N1−104.5 (2)
N1—C1—C2—C3169.4 (3)O7—Mn1—O1—N1−46.0 (3)
O2—C1—C2—C7169.7 (3)O13—Mn1—O1—N1169.2 (2)
N1—C1—C2—C7−10.8 (5)O17—Mn1—O1—N158.3 (2)
C7—C2—C3—C40.2 (5)O4—Mn1—O1—N1−16.5 (2)
C1—C2—C3—C4−180.0 (3)O10—Mn1—O1—N1124.5 (2)
C2—C3—C4—C5−0.7 (6)O18—Mn1—O1—Mn369.81 (15)
C3—C4—C5—C60.1 (6)O7—Mn1—O1—Mn3128.34 (16)
C4—C5—C6—C71.1 (7)O13—Mn1—O1—Mn3−16.45 (13)
C5—C6—C7—O3179.9 (4)O17—Mn1—O1—Mn3−127.38 (14)
C5—C6—C7—C2−1.6 (6)O4—Mn1—O1—Mn3157.78 (15)
C3—C2—C7—O3179.3 (3)O10—Mn1—O1—Mn3−61.2 (2)
C1—C2—C7—O3−0.5 (5)N1—C1—O2—Mn3−1.7 (4)
C3—C2—C7—C61.0 (5)C2—C1—O2—Mn3177.8 (2)
C1—C2—C7—C6−178.9 (3)O15—Mn3—O2—C1−175.9 (2)
O5—C8—C9—C10−0.4 (5)O1—Mn3—O2—C14.1 (2)
N2—C8—C9—C10−179.7 (3)O21—Mn3—O2—C1−87.9 (2)
O5—C8—C9—C14−179.3 (4)O20—Mn3—O2—C193.4 (2)
N2—C8—C9—C141.3 (6)C6—C7—O3—Mn2−156.9 (3)
C14—C9—C10—C11−0.2 (6)C2—C7—O3—Mn224.7 (5)
C8—C9—C10—C11−179.2 (4)N1—Mn2—O3—C7−27.0 (3)
C9—C10—C11—C12−0.8 (7)N6—Mn2—O3—C7162.5 (3)
C10—C11—C12—C131.0 (8)O5—Mn2—O3—C771.3 (3)
C11—C12—C13—C14−0.3 (8)O16—Mn2—O3—C7−115.0 (3)
C12—C13—C14—O6180.0 (5)C8—N2—O4—Mn2−9.1 (4)
C12—C13—C14—C9−0.7 (7)Mn6—N2—O4—Mn2174.45 (13)
C10—C9—C14—O6−179.7 (4)C8—N2—O4—Mn1134.8 (3)
C8—C9—C14—O6−0.8 (6)Mn6—N2—O4—Mn1−41.7 (2)
C10—C9—C14—C130.9 (6)N1—Mn2—O4—N2107.9 (2)
C8—C9—C14—C13179.9 (4)N6—Mn2—O4—N2−81.5 (2)
O8—C15—C16—C17−5.5 (5)O5—Mn2—O4—N29.5 (2)
N3—C15—C16—C17172.5 (3)O16—Mn2—O4—N2−164.0 (2)
O8—C15—C16—C21176.9 (3)N1—Mn2—O4—Mn1−33.59 (14)
N3—C15—C16—C21−5.2 (5)N6—Mn2—O4—Mn1137.00 (14)
C21—C16—C17—C181.0 (6)O5—Mn2—O4—Mn1−131.95 (14)
C15—C16—C17—C18−176.8 (4)O16—Mn2—O4—Mn154.47 (13)
C16—C17—C18—C19−0.6 (6)O18—Mn1—O4—N2−18.3 (2)
C17—C18—C19—C20−0.1 (7)O7—Mn1—O4—N252.54 (19)
C18—C19—C20—C210.5 (7)O13—Mn1—O4—N2−98.9 (3)
C19—C20—C21—O9−179.2 (4)O1—Mn1—O4—N2−111.8 (2)
C19—C20—C21—C16−0.1 (6)O17—Mn1—O4—N2142.5 (2)
C17—C16—C21—O9178.4 (4)O10—Mn1—O4—N2103.1 (2)
C15—C16—C21—O9−4.0 (6)O18—Mn1—O4—Mn2124.15 (14)
C17—C16—C21—C20−0.6 (5)O7—Mn1—O4—Mn2−165.00 (15)
C15—C16—C21—C20177.1 (3)O13—Mn1—O4—Mn243.5 (3)
O11—C22—C23—C28175.2 (3)O1—Mn1—O4—Mn230.66 (13)
N4—C22—C23—C28−5.0 (5)O17—Mn1—O4—Mn2−75.09 (13)
O11—C22—C23—C24−2.8 (5)O10—Mn1—O4—Mn2−114.44 (14)
N4—C22—C23—C24177.0 (3)N2—C8—O5—Mn27.1 (4)
C28—C23—C24—C250.0 (6)C9—C8—O5—Mn2−172.3 (3)
C22—C23—C24—C25178.0 (4)O3—Mn2—O5—C8171.5 (2)
C23—C24—C25—C26−1.0 (7)O4—Mn2—O5—C8−9.0 (2)
C24—C25—C26—C270.7 (8)N1—Mn2—O5—C8−98.3 (2)
C25—C26—C27—C280.7 (8)N6—Mn2—O5—C882.3 (2)
C26—C27—C28—O12179.9 (5)O16—Mn2—O5—C812.7 (5)
C26—C27—C28—C23−1.7 (7)C13—C14—O6—Mn6−177.0 (3)
C24—C23—C28—O12179.6 (4)C9—C14—O6—Mn63.7 (7)
C22—C23—C28—O121.7 (6)N2—Mn6—O6—C14−4.8 (4)
C24—C23—C28—C271.3 (6)N12—Mn6—O6—C14157.3 (4)
C22—C23—C28—C27−176.6 (4)O8—Mn6—O6—C14−102.0 (4)
O14—C29—C30—C31−17.5 (5)C15—N3—O7—Mn61.3 (3)
N5—C29—C30—C31160.4 (4)Mn5—N3—O7—Mn6174.71 (12)
O14—C29—C30—C35161.5 (3)C15—N3—O7—Mn1−131.1 (2)
N5—C29—C30—C35−20.6 (5)Mn5—N3—O7—Mn142.3 (2)
C35—C30—C31—C321.1 (6)N2—Mn6—O7—N3−97.6 (2)
C29—C30—C31—C32−179.8 (4)N12—Mn6—O7—N3100.4 (2)
C30—C31—C32—C33−1.6 (7)O8—Mn6—O7—N3−1.1 (2)
C31—C32—C33—C340.6 (7)N2—Mn6—O7—Mn136.35 (14)
C32—C33—C34—C350.9 (7)N12—Mn6—O7—Mn1−125.61 (13)
C33—C34—C35—O15−178.8 (4)O8—Mn6—O7—Mn1132.89 (13)
C33—C34—C35—C30−1.4 (6)O18—Mn1—O7—N3−178.4 (2)
C31—C30—C35—O15177.7 (4)O13—Mn1—O7—N3−107.6 (2)
C29—C30—C35—O15−1.3 (6)O1—Mn1—O7—N3117.4 (2)
C31—C30—C35—C340.3 (5)O17—Mn1—O7—N38.9 (2)
C29—C30—C35—C34−178.7 (3)O4—Mn1—O7—N387.8 (2)
N6—C41—C42—N70.0 (5)O10—Mn1—O7—N3−55.9 (2)
N8—C46—C47—N9−0.9 (5)O18—Mn1—O7—Mn646.38 (12)
N10—C51—C52—N110.2 (5)O13—Mn1—O7—Mn6117.25 (12)
N12—C56—C57—N130.4 (5)O1—Mn1—O7—Mn6−17.7 (2)
O2—C1—N1—O1−3.1 (5)O17—Mn1—O7—Mn6−126.28 (13)
C2—C1—N1—O1177.4 (3)O4—Mn1—O7—Mn6−47.40 (12)
O2—C1—N1—Mn2178.8 (2)O10—Mn1—O7—Mn6168.91 (14)
C2—C1—N1—Mn2−0.7 (5)N3—C15—O8—Mn6−0.2 (4)
O3—Mn2—N1—C115.5 (3)C16—C15—O8—Mn6177.8 (3)
O4—Mn2—N1—C1−161.9 (3)O6—Mn6—O8—C15−175.8 (2)
O5—Mn2—N1—C1−83.5 (3)O7—Mn6—O8—C150.7 (2)
O16—Mn2—N1—C1112.8 (3)N2—Mn6—O8—C1593.6 (2)
O3—Mn2—N1—O1−162.7 (2)N12—Mn6—O8—C15−85.8 (2)
O4—Mn2—N1—O119.9 (2)C20—C21—O9—Mn5−171.4 (3)
O5—Mn2—N1—O198.3 (2)C16—C21—O9—Mn59.6 (6)
O16—Mn2—N1—O1−65.4 (2)N3—Mn5—O9—C21−5.1 (3)
O5—C8—N2—O40.5 (5)N8—Mn5—O9—C21−175.9 (3)
C9—C8—N2—O4179.8 (3)O11—Mn5—O9—C2189.2 (3)
O5—C8—N2—Mn6176.1 (3)O17—Mn5—O9—C21−85.6 (3)
C9—C8—N2—Mn6−4.6 (5)C22—N4—O10—Mn52.3 (3)
O6—Mn6—N2—C85.4 (3)Mn4—N4—O10—Mn5−177.45 (12)
O7—Mn6—N2—C8−172.6 (3)C22—N4—O10—Mn1131.5 (2)
N12—Mn6—N2—C8−73.5 (5)Mn4—N4—O10—Mn1−48.2 (2)
O8—Mn6—N2—C8108.5 (3)N3—Mn5—O10—N492.5 (2)
O6—Mn6—N2—O4−179.0 (2)N8—Mn5—O10—N4−96.8 (2)
O7—Mn6—N2—O43.1 (2)O11—Mn5—O10—N4−1.4 (2)
N12—Mn6—N2—O4102.2 (4)O17—Mn5—O10—N4172.2 (2)
O8—Mn6—N2—O4−75.9 (2)N3—Mn5—O10—Mn1−40.10 (12)
O8—C15—N3—O7−0.7 (5)N8—Mn5—O10—Mn1130.54 (12)
C16—C15—N3—O7−178.7 (3)O11—Mn5—O10—Mn1−134.07 (12)
O8—C15—N3—Mn5−172.3 (2)O17—Mn5—O10—Mn139.53 (9)
C16—C15—N3—Mn59.8 (5)O18—Mn1—O10—N4−21.9 (2)
O9—Mn5—N3—C15−5.0 (3)O7—Mn1—O10—N4−82.4 (2)
O10—Mn5—N3—C15172.0 (3)O13—Mn1—O10—N456.59 (19)
N8—Mn5—N3—C1559.0 (8)O1—Mn1—O10—N4102.9 (2)
O11—Mn5—N3—C15−109.8 (3)O17—Mn1—O10—N4−176.7 (2)
O17—Mn5—N3—C15105.2 (3)O4—Mn1—O10—N4−133.45 (19)
O9—Mn5—N3—O7−176.6 (2)O18—Mn1—O10—Mn5111.30 (12)
O10—Mn5—N3—O70.4 (2)O7—Mn1—O10—Mn550.83 (11)
N8—Mn5—N3—O7−112.6 (7)O13—Mn1—O10—Mn5−170.19 (13)
O11—Mn5—N3—O778.6 (2)O1—Mn1—O10—Mn5−123.89 (13)
O17—Mn5—N3—O7−66.4 (2)O17—Mn1—O10—Mn5−43.50 (11)
O11—C22—N4—O10−1.9 (5)O4—Mn1—O10—Mn5−0.23 (17)
C23—C22—N4—O10178.3 (3)N4—C22—O11—Mn50.7 (4)
O11—C22—N4—Mn4177.7 (2)C23—C22—O11—Mn5−179.5 (3)
C23—C22—N4—Mn4−2.1 (5)O9—Mn5—O11—C22178.6 (2)
O12—Mn4—N4—C228.5 (3)O10—Mn5—O11—C220.4 (2)
O13—Mn4—N4—C22−172.0 (3)N3—Mn5—O11—C22−92.0 (2)
O19—Mn4—N4—C22−84.4 (3)N8—Mn5—O11—C2290.0 (2)
N10—Mn4—N4—C2299.4 (3)O17—Mn5—O11—C22−9.9 (3)
O12—Mn4—N4—O10−171.8 (2)C27—C28—O12—Mn4−172.5 (3)
O13—Mn4—N4—O107.6 (2)C23—C28—O12—Mn49.2 (6)
O19—Mn4—N4—O1095.3 (2)O14—Mn4—O12—C28165.5 (3)
N10—Mn4—N4—O10−81.0 (2)N4—Mn4—O12—C28−11.7 (3)
O14—C29—N5—O13−3.1 (5)O19—Mn4—O12—C2880.6 (3)
C30—C29—N5—O13179.1 (3)N10—Mn4—O12—C28−102.2 (3)
O14—C29—N5—Mn3−176.0 (2)C29—N5—O13—Mn410.3 (3)
C30—C29—N5—Mn36.2 (5)Mn3—N5—O13—Mn4−175.95 (13)
O15—Mn3—N5—C2918.5 (3)C29—N5—O13—Mn1141.0 (2)
O1—Mn3—N5—C29−161.5 (3)Mn3—N5—O13—Mn1−45.3 (3)
O21—Mn3—N5—C29−69.6 (3)O14—Mn4—O13—N5−10.41 (19)
O20—Mn3—N5—C29109.4 (3)N4—Mn4—O13—N5166.7 (2)
O15—Mn3—N5—O13−154.2 (2)O19—Mn4—O13—N574.57 (19)
O1—Mn3—N5—O1325.8 (2)N10—Mn4—O13—N5−102.8 (2)
O21—Mn3—N5—O13117.7 (2)O14—Mn4—O13—Mn1−143.30 (13)
O20—Mn3—N5—O13−63.2 (2)N4—Mn4—O13—Mn133.85 (13)
N7—C40—N6—C41−0.6 (5)O19—Mn4—O13—Mn1−58.32 (12)
N7—C40—N6—Mn2−168.5 (3)N10—Mn4—O13—Mn1124.28 (13)
C42—C41—N6—C400.4 (5)O18—Mn1—O13—N5−59.8 (2)
C42—C41—N6—Mn2168.7 (3)O7—Mn1—O13—N5−123.33 (19)
O3—Mn2—N6—C40−172.3 (3)O1—Mn1—O13—N534.06 (19)
O4—Mn2—N6—C405.2 (3)O17—Mn1—O13—N5132.40 (19)
O5—Mn2—N6—C40−73.2 (3)O4—Mn1—O13—N521.3 (3)
O16—Mn2—N6—C4090.3 (3)O10—Mn1—O13—N5−175.6 (2)
O3—Mn2—N6—C4121.9 (3)O18—Mn1—O13—Mn469.93 (12)
O4—Mn2—N6—C41−160.7 (3)O7—Mn1—O13—Mn46.37 (17)
O5—Mn2—N6—C41120.9 (3)O1—Mn1—O13—Mn4163.76 (13)
O16—Mn2—N6—C41−75.5 (3)O17—Mn1—O13—Mn4−97.90 (12)
N6—C40—N7—C420.6 (5)O4—Mn1—O13—Mn4150.97 (16)
N6—C40—N7—C43179.2 (4)O10—Mn1—O13—Mn4−45.91 (11)
C41—C42—N7—C40−0.3 (5)N5—C29—O14—Mn4−5.9 (4)
C41—C42—N7—C43−178.9 (4)C30—C29—O14—Mn4171.9 (3)
C44—C43—N7—C40−115.0 (5)O12—Mn4—O14—C29−171.6 (2)
C44—C43—N7—C4263.3 (6)O13—Mn4—O14—C299.0 (2)
N9—C45—N8—C46−0.6 (4)O19—Mn4—O14—C29−79.2 (2)
N9—C45—N8—Mn5−178.3 (2)N10—Mn4—O14—C2997.3 (2)
C47—C46—N8—C451.0 (5)C34—C35—O15—Mn3−145.4 (3)
C47—C46—N8—Mn5178.6 (3)C30—C35—O15—Mn337.3 (5)
O9—Mn5—N8—C45−11.8 (3)O2—Mn3—O15—C35142.7 (3)
O10—Mn5—N8—C45170.9 (3)N5—Mn3—O15—C35−39.5 (3)
N3—Mn5—N8—C45−75.9 (8)O21—Mn3—O15—C3553.3 (3)
O11—Mn5—N8—C4592.9 (3)O20—Mn3—O15—C35−128.9 (3)
O17—Mn5—N8—C45−121.5 (3)O17—C36—O16—Mn2−69.2 (4)
O9—Mn5—N8—C46171.0 (3)C37—C36—O16—Mn2109.6 (4)
O10—Mn5—N8—C46−6.3 (3)O3—Mn2—O16—C36−159.1 (3)
N3—Mn5—N8—C46106.9 (7)O4—Mn2—O16—C3621.2 (3)
O11—Mn5—N8—C46−84.3 (3)N1—Mn2—O16—C36112.3 (3)
O17—Mn5—N8—C4661.3 (3)N6—Mn2—O16—C36−71.0 (3)
N8—C45—N9—C470.0 (4)O5—Mn2—O16—C36−0.2 (5)
N8—C45—N9—C48−178.5 (4)O16—C36—O17—Mn128.4 (5)
C46—C47—N9—C450.5 (5)C37—C36—O17—Mn1−150.5 (3)
C46—C47—N9—C48179.1 (4)O16—C36—O17—Mn5168.0 (2)
C49—C48—N9—C4584.9 (6)C37—C36—O17—Mn5−10.9 (5)
C49—C48—N9—C47−93.4 (7)O18—Mn1—O17—C3691.3 (4)
N11—C50—N10—C510.0 (5)O7—Mn1—O17—C36109.4 (3)
N11—C50—N10—Mn4173.7 (2)O13—Mn1—O17—C36−121.3 (3)
C52—C51—N10—C50−0.1 (5)O1—Mn1—O17—C36−39.6 (3)
C52—C51—N10—Mn4−173.4 (3)O4—Mn1—O17—C3633.9 (3)
O12—Mn4—N10—C5025.9 (3)O10—Mn1—O17—C36−177.1 (3)
O13—Mn4—N10—C50−156.6 (3)O18—Mn1—O17—Mn5−60.1 (3)
O14—Mn4—N10—C50121.3 (3)O7—Mn1—O17—Mn5−42.05 (9)
N4—Mn4—N10—C50−63.4 (3)O13—Mn1—O17—Mn587.31 (10)
O12—Mn4—N10—C51−162.1 (4)O1—Mn1—O17—Mn5168.97 (8)
O13—Mn4—N10—C5115.5 (4)O4—Mn1—O17—Mn5−117.57 (9)
O14—Mn4—N10—C51−66.7 (4)O10—Mn1—O17—Mn531.44 (8)
N4—Mn4—N10—C51108.6 (4)O9—Mn5—O17—C36−3.4 (3)
N10—C50—N11—C520.1 (5)O10—Mn5—O17—C36174.4 (3)
N10—C50—N11—C53−179.5 (4)N3—Mn5—O17—C36−88.5 (3)
C51—C52—N11—C50−0.2 (5)N8—Mn5—O17—C3684.1 (3)
C51—C52—N11—C53179.5 (4)O11—Mn5—O17—C36−174.7 (3)
C54—C53—N11—C507.8 (7)O9—Mn5—O17—Mn1144.91 (10)
C54—C53—N11—C52−171.7 (5)O10—Mn5—O17—Mn1−37.27 (9)
N13—C55—N12—C56−0.5 (5)N3—Mn5—O17—Mn159.80 (11)
N13—C55—N12—Mn6173.6 (3)N8—Mn5—O17—Mn1−127.52 (11)
C57—C56—N12—C550.0 (5)O11—Mn5—O17—Mn1−26.3 (2)
C57—C56—N12—Mn6−174.0 (3)O19—C38—O18—Mn1−4.8 (5)
O6—Mn6—N12—C55−167.2 (3)C39—C38—O18—Mn1177.2 (3)
O7—Mn6—N12—C5511.9 (3)O7—Mn1—O18—C3894.9 (3)
N2—Mn6—N12—C55−88.1 (5)O13—Mn1—O18—C38−36.2 (3)
O8—Mn6—N12—C5590.0 (3)O1—Mn1—O18—C38−113.7 (3)
O6—Mn6—N12—C565.7 (3)O17—Mn1—O18—C38114.0 (3)
O7—Mn6—N12—C56−175.2 (3)O4—Mn1—O18—C38169.7 (3)
N2—Mn6—N12—C5684.8 (5)O10—Mn1—O18—C3833.0 (3)
O8—Mn6—N12—C56−97.1 (3)O18—C38—O19—Mn424.7 (6)
N12—C55—N13—C570.7 (5)C39—C38—O19—Mn4−157.2 (3)
N12—C55—N13—C58−172.8 (4)O12—Mn4—O19—C38−171.1 (4)
C56—C57—N13—C55−0.7 (5)O13—Mn4—O19—C3811.4 (4)
C56—C57—N13—C58172.9 (4)O14—Mn4—O19—C3893.8 (4)
C59—C58—N13—C5586.8 (6)N4—Mn4—O19—C38−81.7 (4)
C59—C58—N13—C57−85.5 (6)N14—C60—O20—Mn3−177.5 (3)
O20—C60—N14—C610.6 (7)O15—Mn3—O20—C60170.4 (3)
O20—C60—N14—C62178.9 (4)O1—Mn3—O20—C60−10.2 (3)
O22—C66—N16—C67−4.0 (11)O2—Mn3—O20—C60−92.2 (3)
O22—C66—N16—C68179.6 (7)N5—Mn3—O20—C6080.3 (3)
C1—N1—O1—Mn36.3 (3)O15—Mn3—O21—C63−178.8 (4)
Mn2—N1—O1—Mn3−175.27 (12)O1—Mn3—O21—C631.9 (4)
C1—N1—O1—Mn1−178.9 (2)O2—Mn3—O21—C6383.8 (4)
Mn2—N1—O1—Mn1−0.5 (3)N5—Mn3—O21—C63−88.7 (4)
O2—Mn3—O1—N1−5.57 (19)Mn3—O21—C63—N15178.0 (3)
N5—Mn3—O1—N1176.7 (2)O21—C63—N15—C640.4 (6)
O21—Mn3—O1—N183.8 (2)O21—C63—N15—C65176.6 (4)
O20—Mn3—O1—N1−94.0 (2)C72—O26—C70—C71−171.7 (17)
O2—Mn3—O1—Mn1179.45 (15)C70—O26—C72—C73−74 (2)
N5—Mn3—O1—Mn11.69 (15)C72B—O26B—C70B—C71B169 (2)
O21—Mn3—O1—Mn1−91.16 (14)C70B—O26B—C72B—C73B177 (2)
O20—Mn3—O1—Mn191.03 (14)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O24—H24A···O220.842.092.876 (7)156
O24B—H24B···O190.842.152.98 (2)170
O25—H25A···O24B0.84 (2)2.35 (2)3.05 (4)140 (6)
O25—H25B···O220.84 (2)1.99 (2)2.776 (17)156 (4)

Experimental details

Crystal data
Chemical formula[Mn6(C7H4NO3)5(C2H3O2)2(C5H8N2)4(C3H7NO)2]·C4H10O·C3H7NO·CH4O·0.12H2O
Mr1910.51
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)12.604 (2), 17.188 (3), 20.990 (4)
α, β, γ (°)103.564 (3), 97.322 (3), 107.658 (3)
V (Å3)4114.2 (13)
Z2
Radiation typeMo Kα
µ (mm−1)0.98
Crystal size (mm)0.35 × 0.29 × 0.13
Data collection
DiffractometerBruker SMART APEX CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2009)
Tmin, Tmax0.563, 0.746
No. of measured, independent and
observed [I > 2σ(I)] reflections		49270, 18692, 14786
Rint0.046
(sin θ/λ)max (Å−1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.059, 0.148, 1.07
No. of reflections18692
No. of parameters1143
No. of restraints53
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å−3)1.53, −0.76

Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXTL (Sheldrick, 2008), Mercury (Macrae et al., 2006) and ORTEP-3 (Farrugia, 1997).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O24—H24A···O220.842.092.876 (7)155.7
O24B—H24B···O190.842.152.98 (2)169.7
O25—H25A···O24B0.84 (2)2.35 (2)3.05 (4)140 (6)
O25—H25B···O220.835 (18)1.991 (18)2.776 (17)156 (4)
 

Acknowledgements

This work was funded by the Shippensburg University CFEST Teaching and Research Excellence Program and the Shippensburg University Foundation (grant No. UG 2540–10) to BRT and CMZ. The diffractometer was funded by NSF grant No. 0087210, by Ohio Board of Regents grant No. CAP-491, and by YSU.

References

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Journal logoCRYSTALLOGRAPHIC
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ISSN: 2056-9890
Volume 67| Part 8| August 2011| Pages m1041-m1042
doi:10.1107/S160053681102602X
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