Literature DB >> 21754606

catena-Poly[[[tetra-kis-(cyanido-κC)tungstate(IV)]-di-μ-cyanido-κC:N-bis-[diaqua-(2,2'-bipyridyl-κN,N')manganese(II)]-di-μ-cyanido-κN:C] hexa-hydrate].

Noriaki Ozaki1, Ryo Yamada, Koji Nakabayashi, Shin-Ichi Ohkoshi.   

Abstract

The polymeric title compound, {[Mn(II) (2)W(IV)(CN)(8)(C(10)H(8)N(2))(2)(H(2)O)(4)]·6H(2)O}(n), has a one-dimensional cyanide-bridged Mn(II)-W(IV) bimetallic assembly. The coordination geometry of the W(IV) atom is eight-coordinate square-anti-prismatic and that of each of the Mn(II) atoms is six-coordinate distorted octa-hedral. Two pairs of CN ligands of W(CN)(8) are bridged to two Mn(II) atoms, the remaining CN ligands being terminal. Each Mn(II) atom is additionally coordinated by a bidentate 2,2'-bipyridyl ligand and two water mol-ecules. The crystal structure is stabilized by O-H⋯O and O-H⋯N hydrogen bonds.

Entities:  

Year:  2011        PMID： 21754606      PMCID： PMC3120535          DOI： 10.1107/S1600536811012451

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For general background to octa­cyanido­tungstates as magnetic materials, see: Ohkoshi et al. (2007 ▶, 2008 ▶); Sieklucka et al. (2009 ▶). For related octa­cyanido­tungstate structures, see: Herrera et al. (2003 ▶); Leipoldt et al. (1994 ▶); Sieklucka et al. (2000 ▶).

Experimental

Crystal data

[Mn2W(CN)8(C10H8N2)2(H2O)4]·6H2O M = 992.40 Monoclinic, a = 11.6673 (3) Å b = 15.5511 (4) Å c = 21.4339 (7) Å β = 99.213 (1)° V = 3838.78 (18) Å3 Z = 4 Mo Kα radiation μ = 3.70 mm−1 T = 90 K 0.90 × 0.20 × 0.02 mm

Data collection

Rigaku R-AXIS RAPID diffractometer Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.135, T max = 0.930 33108 measured reflections 8606 independent reflections 7342 reflections with I > 2σ(I) R int = 0.062

Refinement

R[F 2 > 2σ(F 2)] = 0.036 wR(F 2) = 0.079 S = 1.03 8606 reflections 533 parameters 18 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 2.47 e Å−3 Δρmin = −1.92 e Å−3 Data collection: PROCESS-AUTO (Rigaku, 2007 ▶); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Molecular Structure Corporation & Rigaku, 2007 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶) and VESTA (Momma & Izumi, 2006 ▶); software used to prepare material for publication: CrystalStructure. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811012451/tk2734sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536811012451/tk2734Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Mn2W(CN)8(C10H8N2)2(H2O)4]·6H2OF(000) = 1960
Mr = 992.40Dx = 1.717 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71075 Å
Hall symbol: -P 2ynCell parameters from 28294 reflections
a = 11.6673 (3) Åθ = 3.1–27.5°
b = 15.5511 (4) ŵ = 3.70 mm−1
c = 21.4339 (7) ÅT = 90 K
β = 99.213 (1)°Platelet, yellow
V = 3838.78 (18) Å30.90 × 0.20 × 0.02 mm
Z = 4
Rigaku R-AXIS RAPID diffractometer8606 independent reflections
Radiation source: fine-focus sealed tube7342 reflections with I > 2σ(I)
graphiteRint = 0.062
Detector resolution: 10.00 pixels mm-1θmax = 27.5°, θmin = 3.1°
ω scansh = −15→15
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)k = −18→19
Tmin = 0.135, Tmax = 0.930l = −27→27
33108 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.079H atoms treated by a mixture of independent and constrained refinement
S = 1.03w = 1/[σ2(Fo2) + (0.0278P)2 + 5.0172P] where P = (Fo2 + 2Fc2)/3
8606 reflections(Δ/σ)max = 0.002
533 parametersΔρmax = 2.47 e Å−3
18 restraintsΔρmin = −1.92 e Å−3
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.Bond lengths and angles W1 - Distance Angles C2 2.1424 (0.0041) C4 2.1437 (0.0038) 107.63 (0.14) C3 2.1494 (0.0039) 76.34 (0.14) 142.60 (0.13) C1 2.1498 (0.0038) 142.96 (0.14) 84.20 (0.13) 73.85 (0.14) C7 2.1591 (0.0039) 84.55 (0.15) 145.08 (0.14) 71.42 (0.14) 105.89 (0.14) C8 2.1700 (0.0040) 73.08 (0.15) 71.85 (0.14) 74.17 (0.14) 78.01 (0.14) 142.45 (0.15) C6 2.1858 (0.0040) 70.17 (0.14) 75.29 (0.14) 136.71 (0.14) 146.11 (0.14) 78.73 (0.14) 119.10 (0.14) C5 2.1872 (0.0040) 143.73 (0.14) 75.60 (0.13) 123.59 (0.13) 72.70 (0.14) 75.84 (0.14) 137.85 (0.14) 76.19 (0.13) W1 - C2 C4 C3 C1 C7 C8 C6 Mn1 - Distance Angles N2_$1 2.1508 (0.0033) N1 2.1762 (0.0033) 96.57 (0.13) O2 2.2209 (0.0030) 82.20 (0.12) 169.50 (0.12) N10 2.2339 (0.0032) 93.95 (0.12) 89.84 (0.12) 100.64 (0.12) O1 2.2440 (0.0029) 92.57 (0.12) 81.90 (0.12) 87.73 (0.12) 170.02 (0.12) N9 2.2542 (0.0029) 159.83 (0.12) 99.14 (0.12) 84.59 (0.11) 73.59 (0.11) 102.08 (0.11) Mn1 - N2_$1 N1 O2 N10 O1 Mn2 - Distance Angles N3 2.1504 (0.0032) N4_$4 2.2012 (0.0032) 92.55 (0.12) O4 2.2194 (0.0030) 83.38 (0.12) 165.86 (0.11) O3 2.2289 (0.0030) 100.21 (0.12) 83.18 (0.11) 84.22 (0.11) N12 2.2482 (0.0030) 93.06 (0.12) 91.00 (0.11) 102.71 (0.11) 165.71 (0.12) N11 2.2493 (0.0032) 162.59 (0.12) 98.25 (0.12) 89.14 (0.11) 94.61 (0.12) 73.24 (0.12) Mn2 - N3 N4_$4 O4 O3 N12 O1 - Distance Angles Mn1 2.2440 (0.0029) H1 0.8363 (0.0190) 108.96 (3.32) H2 0.8417 (0.0190) 110.06 (3.33) 105.52 (4.66) O1 - Mn1 H1 O2 - Distance Angles Mn1 2.2209 (0.0030) H3 0.8337 (0.0190) 132.79 (3.41) H4 0.8222 (0.0191) 120.69 (3.30) 105.61 (4.59) O2 - Mn1 H3 O3 - Distance Angles Mn2 2.2289 (0.0030) H5 0.8240 (0.0190) 109.88 (3.40) H6 0.8286 (0.0191) 118.44 (3.40) 104.60 (4.67) O3 - Mn2 H5 O4 - Distance Angles Mn2 2.2194 (0.0030) H7 0.8366 (0.0189) 120.24 (3.34) H8 0.8296 (0.0189) 114.26 (3.19) 104.47 (4.45) O4 - Mn2 H7 O5 - Distance Angles H29 0.8350 (0.0192) H30 0.8362 (0.0193) 107.18 (4.93) O5 - H29 O6 - Distance Angles H31 0.8332 (0.0191) H32 0.8267 (0.0188) 113.94 (4.49) O6 - H31 O7 - Distance Angles H33 0.8258 (0.0190) H34 0.8236 (0.0189) 104.31 (4.54) O7 - H33 O8 - Distance Angles H36 0.8307 (0.0193) H35 0.8285 (0.0194) 113.61 (5.07) O8 - H36 O9 - Distance Angles H37 0.8344 (0.0189) H38 0.8390 (0.0192) 111.00 (4.58) O9 - H37 N1 - Distance Angles C1 1.1627 (0.0048) Mn1 2.1762 (0.0033) 158.65 (0.31) N1 - C1 N2 - Distance Angles C2 1.1582 (0.0051) Mn1_$4 2.1508 (0.0033) 159.78 (0.31) N2 - C2 N3 - Distance Angles C3 1.1545 (0.0048) Mn2 2.1504 (0.0032) 176.05 (0.31) N3 - C3 N4 - Distance Angles C4 1.1529 (0.0047) Mn2_$1 2.2011 (0.0032) 146.40 (0.30) N4 - C4 N5 - Distance Angles C5 1.1465 (0.0049) N5 - N6 - Distance Angles C6 1.1526 (0.0051) N6 - N7 - Distance Angles C7 1.1597 (0.0050) N7 - N8 - Distance Angles C8 1.1575 (0.0052) N8 - N9 - Distance Angles C9 1.3429 (0.0050) C13 1.3559 (0.0045) 118.44 (0.31) Mn1 2.2542 (0.0029) 124.73 (0.24) 116.59 (0.24) N9 - C9 C13 N10 - Distance Angles C18 1.3462 (0.0050) C14 1.3514 (0.0048) 118.82 (0.33) Mn1 2.2339 (0.0032) 123.80 (0.25) 117.30 (0.25) N10 - C18 C14 N11 - Distance Angles C19 1.3327 (0.0053) C23 1.3506 (0.0048) 119.05 (0.34) Mn2 2.2493 (0.0032) 124.16 (0.27) 116.66 (0.26) N11 - C19 C23 N12 - Distance Angles C28 1.3420 (0.0050) C24 1.3487 (0.0048) 118.53 (0.32) Mn2 2.2482 (0.0030) 124.07 (0.25) 117.37 (0.25) N12 - C28 C24 C1 - Distance Angles N1 1.1627 (0.0048) W1 2.1498 (0.0038) 178.55 (0.34) C1 - N1 C2 - Distance Angles N2 1.1582 (0.0051) W1 2.1424 (0.0041) 177.68 (0.34) C2 - N2 C3 - Distance Angles N3 1.1545 (0.0048) W1 2.1494 (0.0039) 178.65 (0.34) C3 - N3 C4 - Distance Angles N4 1.1529 (0.0047) W1 2.1437 (0.0038) 175.63 (0.33) C4 - N4 C5 - Distance Angles N5 1.1465 (0.0049) W1 2.1872 (0.0039) 176.70 (0.31) C5 - N5 C6 - Distance Angles N6 1.1526 (0.0051) W1 2.1858 (0.0040) 177.03 (0.32) C6 - N6 C7 - Distance Angles N7 1.1597 (0.0050) W1 2.1591 (0.0039) 178.24 (0.37) C7 - N7 C8 - Distance Angles N8 1.1575 (0.0052) W1 2.1700 (0.0040) 178.82 (0.38) C8 - N8 C9 - Distance Angles N9 1.3429 (0.0050) C10 1.3907 (0.0053) 123.11 (0.36) H9 0.9500 118.44 118.44 C9 - N9 C10 C10 - Distance Angles C11 1.3817 (0.0057) C9 1.3907 (0.0053) 117.87 (0.37) H10 0.9500 121.07 121.07 C10 - C11 C9 C11 - Distance Angles C10 1.3817 (0.0057) C12 1.3945 (0.0060) 119.57 (0.36) H11 0.9500 120.22 120.22 C11 - C10 C12 C12 - Distance Angles C13 1.3781 (0.0052) C11 1.3945 (0.0060) 119.19 (0.36) H12 0.9500 120.41 120.41 C12 - C13 C11 C13 - Distance Angles N9 1.3559 (0.0045) C12 1.3781 (0.0052) 121.72 (0.36) C14 1.4931 (0.0055) 115.99 (0.32) 122.28 (0.35) C13 - N9 C12 C14 - Distance Angles N10 1.3514 (0.0048) C15 1.3977 (0.0051) 121.38 (0.36) C13 1.4931 (0.0054) 116.37 (0.32) 122.22 (0.35) C14 - N10 C15 C15 - Distance Angles C16 1.3876 (0.0061) C14 1.3977 (0.0051) 119.00 (0.38) H15 0.9500 120.50 120.50 C15 - C16 C14 C16 - Distance Angles C17 1.3835 (0.0060) C15 1.3876 (0.0061) 119.36 (0.37) H16 0.9500 120.32 120.32 C16 - C17 C15 C17 - Distance Angles C18 1.3809 (0.0054) C16 1.3835 (0.0060) 118.75 (0.39) H17 0.9500 120.63 120.63 C17 - C18 C16 C18 - Distance Angles N10 1.3462 (0.0049) C17 1.3809 (0.0054) 122.69 (0.37) H18 0.9500 118.66 118.66 C18 - N10 C17 C19 - Distance Angles N11 1.3327 (0.0053) C20 1.3846 (0.0058) 122.88 (0.42) H19 0.9500 118.56 118.56 C19 - N11 C20 C20 - Distance Angles C21 1.3833 (0.0064) C19 1.3846 (0.0058) 118.35 (0.44) H20 0.9500 120.82 120.82 C20 - C21 C19 C21 - Distance Angles C22 1.3743 (0.0066) C20 1.3833 (0.0064) 119.29 (0.40) H21 0.9500 120.36 120.36 C21 - C22 C20 C22 - Distance Angles C21 1.3743 (0.0066) C23 1.3955 (0.0055) 119.60 (0.41) H22 0.9500 120.20 120.20 C22 - C21 C23 C23 - Distance Angles N11 1.3506 (0.0048) C22 1.3955 (0.0055) 120.82 (0.38) C24 1.4917 (0.0058) 116.51 (0.33) 122.62 (0.37) C23 - N11 C22 C24 - Distance Angles N12 1.3487 (0.0048) C25 1.3938 (0.0054) 121.71 (0.39) C23 1.4917 (0.0058) 115.76 (0.33) 122.50 (0.37) C24 - N12 C25 C25 - Distance Angles C26 1.3784 (0.0067) C24 1.3938 (0.0054) 118.98 (0.40) H25 0.9500 120.51 120.51 C25 - C26 C24 C26 - Distance Angles C25 1.3784 (0.0067) C27 1.3910 (0.0061) 119.72 (0.39) H26 0.9500 120.14 120.14 C26 - C25 C27 C27 - Distance Angles C28 1.3840 (0.0053) C26 1.3910 (0.0061) 117.90 (0.40) H27 0.9500 121.05 121.05 C27 - C28 C26 C28 - Distance Angles N12 1.3420 (0.0050) C27 1.3840 (0.0053) 123.16 (0.37) H28 0.9500 118.42 118.42 C28 - N12 C27
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.
xyzUiso*/Ueq
W10.810420 (12)0.888675 (9)0.224158 (6)0.01102 (6)
Mn10.45358 (5)1.11286 (4)0.17557 (3)0.01337 (12)
Mn20.47767 (5)0.64730 (4)0.15037 (2)0.01383 (12)
O10.4226 (3)1.0759 (2)0.27269 (13)0.0256 (7)
H10.487 (2)1.069 (3)0.2960 (19)0.031*
H20.390 (4)1.116 (2)0.289 (2)0.031*
O20.3345 (2)1.2232 (2)0.18036 (15)0.0263 (7)
H30.2623 (17)1.227 (3)0.175 (2)0.032*
H40.359 (4)1.2694 (18)0.196 (2)0.032*
O30.4296 (3)0.6143 (2)0.24405 (14)0.0256 (7)
H50.482 (3)0.586 (3)0.265 (2)0.031*
H60.417 (4)0.654 (2)0.2679 (18)0.031*
O40.3504 (2)0.7532 (2)0.15113 (13)0.0233 (6)
H70.281 (2)0.742 (3)0.154 (2)0.028*
H80.370 (4)0.790 (2)0.1789 (17)0.028*
O51.1463 (3)1.3841 (2)0.25177 (16)0.0298 (7)
H291.110 (4)1.4308 (19)0.249 (2)0.036*
H301.217 (2)1.396 (3)0.253 (2)0.036*
O61.1027 (3)1.24366 (19)0.17341 (14)0.0254 (7)
H311.096 (4)1.288 (2)0.1945 (19)0.030*
H321.055 (3)1.240 (3)0.1406 (14)0.030*
O70.9086 (3)1.22249 (19)0.08148 (14)0.0233 (6)
H330.898 (4)1.1743 (17)0.096 (2)0.028*
H340.866 (3)1.254 (3)0.0984 (19)0.028*
O80.9834 (3)1.2948 (2)−0.02763 (16)0.0358 (8)
H360.956 (4)1.274 (3)0.0026 (17)0.043*
H351.035 (3)1.265 (3)−0.039 (2)0.043*
O90.8777 (3)1.2844 (2)−0.14985 (14)0.0283 (7)
H370.901 (4)1.298 (3)−0.1123 (11)0.034*
H380.913 (4)1.241 (2)−0.160 (2)0.034*
O100.8624 (3)0.5937 (3)0.14671 (17)0.0539 (11)
N10.5679 (3)1.0016 (2)0.18906 (15)0.0190 (7)
N20.9176 (3)0.7068 (2)0.28805 (16)0.0213 (7)
N30.6026 (3)0.7475 (2)0.17782 (14)0.0175 (7)
N40.8920 (3)1.0454 (2)0.32493 (14)0.0178 (7)
N50.8726 (3)1.0573 (2)0.13964 (15)0.0204 (7)
N61.1000 (3)0.8869 (2)0.24367 (16)0.0223 (8)
N70.8601 (3)0.7988 (2)0.09063 (16)0.0277 (8)
N80.6807 (3)0.8526 (2)0.34906 (16)0.0286 (8)
N90.3003 (3)1.0525 (2)0.11361 (13)0.0148 (7)
N100.4871 (3)1.1251 (2)0.07622 (15)0.0166 (7)
N110.3369 (3)0.5667 (2)0.09489 (15)0.0195 (7)
N120.5095 (3)0.6474 (2)0.04966 (14)0.0155 (7)
C10.6537 (3)0.9626 (2)0.20079 (16)0.0144 (8)
C20.8776 (3)0.7701 (3)0.26592 (17)0.0186 (8)
C30.6743 (3)0.7977 (3)0.19365 (16)0.0149 (8)
C40.8609 (3)0.9891 (2)0.29147 (16)0.0142 (8)
C50.8501 (3)0.9979 (3)0.16697 (16)0.0145 (8)
C61.0001 (3)0.8900 (2)0.23681 (17)0.0163 (8)
C70.8414 (3)0.8311 (3)0.13671 (17)0.0180 (8)
C80.7253 (3)0.8661 (3)0.30556 (18)0.0189 (8)
C90.2107 (3)1.0146 (3)0.13495 (18)0.0203 (8)
H90.20541.01960.17860.024*
C100.1254 (3)0.9682 (3)0.09624 (19)0.0234 (9)
H100.06470.94030.11310.028*
C110.1318 (3)0.9641 (3)0.03249 (19)0.0258 (10)
H110.07540.93260.00470.031*
C120.2215 (3)1.0065 (3)0.00926 (18)0.0225 (9)
H120.22471.0065−0.03470.027*
C130.3053 (3)1.0485 (3)0.05091 (17)0.0172 (8)
C140.4080 (3)1.0904 (2)0.03018 (17)0.0156 (8)
C150.4242 (4)1.0915 (3)−0.03304 (18)0.0210 (9)
H150.36751.0673−0.06500.025*
C160.5243 (4)1.1284 (3)−0.04842 (19)0.0257 (10)
H160.53691.1297−0.09110.031*
C170.6054 (4)1.1632 (3)−0.00101 (19)0.0244 (9)
H170.67491.1882−0.01050.029*
C180.5835 (3)1.1609 (3)0.06040 (18)0.0190 (8)
H180.63871.18570.09280.023*
C190.2547 (4)0.5260 (3)0.1201 (2)0.0264 (9)
H190.25840.52740.16470.032*
C200.1643 (4)0.4819 (3)0.0842 (2)0.0325 (11)
H200.10720.45340.10360.039*
C210.1592 (4)0.4803 (3)0.0193 (2)0.0335 (11)
H210.09810.4507−0.00670.040*
C220.2434 (4)0.5220 (3)−0.0073 (2)0.0301 (10)
H220.24050.5219−0.05180.036*
C230.3331 (3)0.5645 (3)0.03160 (18)0.0193 (8)
C240.4317 (4)0.6061 (2)0.00663 (18)0.0183 (8)
C250.4452 (4)0.6007 (3)−0.05668 (19)0.0270 (10)
H250.38920.5717−0.08640.032*
C260.5413 (4)0.6380 (3)−0.0755 (2)0.0296 (10)
H260.55190.6350−0.11850.036*
C270.6226 (4)0.6800 (3)−0.03138 (18)0.0238 (9)
H270.68980.7055−0.04330.029*
C280.6025 (3)0.6833 (3)0.03048 (18)0.0195 (8)
H280.65710.71250.06080.023*
U11U22U33U12U13U23
W10.01106 (9)0.01089 (9)0.01059 (8)0.00028 (6)0.00020 (5)−0.00007 (5)
Mn10.0120 (3)0.0139 (3)0.0135 (3)0.0009 (2)0.0000 (2)−0.0007 (2)
Mn20.0134 (3)0.0148 (3)0.0129 (3)−0.0006 (2)0.0007 (2)−0.0002 (2)
O10.0334 (18)0.0266 (17)0.0183 (15)0.0010 (15)0.0087 (12)−0.0014 (12)
O20.0149 (14)0.0209 (17)0.0412 (18)0.0019 (13)−0.0012 (13)−0.0107 (13)
O30.0317 (17)0.0262 (18)0.0205 (15)0.0088 (14)0.0095 (13)0.0049 (12)
O40.0155 (14)0.0284 (18)0.0263 (16)0.0017 (14)0.0045 (12)−0.0002 (12)
O50.0197 (16)0.0264 (18)0.0425 (19)0.0022 (14)0.0022 (14)−0.0066 (14)
O60.0232 (16)0.0232 (17)0.0286 (17)0.0015 (14)0.0009 (12)−0.0042 (13)
O70.0291 (16)0.0187 (16)0.0238 (15)0.0002 (14)0.0098 (12)0.0006 (12)
O80.0362 (19)0.043 (2)0.0322 (18)0.0063 (17)0.0168 (15)0.0078 (15)
O90.0208 (15)0.036 (2)0.0292 (16)0.0044 (14)0.0079 (13)0.0056 (14)
O100.043 (2)0.082 (3)0.037 (2)−0.024 (2)0.0055 (17)−0.0118 (19)
N10.0197 (17)0.0174 (17)0.0192 (16)0.0025 (15)0.0011 (13)−0.0010 (13)
N20.0149 (16)0.0215 (19)0.0274 (18)0.0006 (15)0.0031 (13)0.0037 (15)
N30.0150 (16)0.0187 (18)0.0184 (16)−0.0007 (15)0.0012 (12)−0.0032 (13)
N40.0216 (17)0.0176 (18)0.0139 (16)−0.0047 (15)0.0016 (13)0.0024 (13)
N50.0264 (18)0.0180 (18)0.0165 (16)−0.0043 (15)0.0024 (13)0.0007 (13)
N60.0191 (19)0.023 (2)0.0252 (18)−0.0017 (15)0.0042 (14)0.0036 (14)
N70.0290 (19)0.031 (2)0.0245 (19)−0.0028 (17)0.0078 (15)−0.0086 (16)
N80.038 (2)0.025 (2)0.0241 (19)−0.0143 (18)0.0110 (16)−0.0029 (15)
N90.0128 (15)0.0194 (18)0.0120 (15)0.0008 (14)0.0014 (12)−0.0004 (12)
N100.0192 (17)0.0133 (17)0.0175 (16)0.0021 (14)0.0034 (13)0.0017 (12)
N110.0170 (16)0.0186 (18)0.0217 (17)0.0005 (15)−0.0010 (13)0.0002 (14)
N120.0174 (16)0.0151 (17)0.0143 (15)0.0025 (14)0.0028 (12)0.0010 (12)
C10.0200 (19)0.0131 (19)0.0106 (17)−0.0020 (17)0.0040 (14)−0.0030 (13)
C20.0145 (19)0.024 (2)0.0165 (19)−0.0045 (17)0.0011 (14)0.0007 (16)
C30.0152 (18)0.016 (2)0.0144 (17)0.0056 (17)0.0052 (14)0.0012 (14)
C40.0108 (17)0.018 (2)0.0143 (18)0.0011 (16)0.0039 (13)0.0022 (15)
C50.0118 (18)0.018 (2)0.0132 (17)−0.0020 (16)0.0003 (13)−0.0056 (15)
C60.021 (2)0.0124 (19)0.0155 (18)0.0018 (16)0.0038 (15)0.0011 (14)
C70.0161 (19)0.019 (2)0.0187 (19)−0.0046 (17)0.0029 (15)0.0002 (16)
C80.022 (2)0.018 (2)0.0163 (19)−0.0001 (17)−0.0004 (16)−0.0009 (15)
C90.020 (2)0.021 (2)0.0195 (19)0.0019 (18)0.0037 (15)0.0003 (16)
C100.0148 (19)0.027 (2)0.028 (2)−0.0047 (18)0.0024 (16)0.0007 (17)
C110.019 (2)0.030 (2)0.026 (2)0.0003 (19)−0.0062 (16)−0.0091 (18)
C120.025 (2)0.025 (2)0.0152 (19)0.0021 (19)−0.0021 (16)−0.0027 (16)
C130.0168 (19)0.017 (2)0.0175 (18)0.0056 (17)−0.0001 (15)0.0015 (15)
C140.0177 (19)0.0133 (19)0.0163 (18)0.0072 (16)0.0041 (14)0.0046 (14)
C150.028 (2)0.020 (2)0.0142 (18)0.0077 (18)0.0037 (16)0.0024 (15)
C160.034 (2)0.025 (2)0.020 (2)0.011 (2)0.0123 (18)0.0064 (17)
C170.025 (2)0.022 (2)0.028 (2)0.0046 (19)0.0121 (17)0.0100 (17)
C180.0126 (18)0.018 (2)0.027 (2)0.0014 (17)0.0049 (15)0.0027 (16)
C190.022 (2)0.025 (2)0.033 (2)−0.0023 (19)0.0067 (18)−0.0006 (18)
C200.022 (2)0.027 (3)0.047 (3)−0.005 (2)0.003 (2)−0.002 (2)
C210.024 (2)0.029 (3)0.043 (3)−0.005 (2)−0.006 (2)−0.007 (2)
C220.033 (2)0.027 (2)0.025 (2)0.005 (2)−0.0101 (19)−0.0022 (18)
C230.022 (2)0.012 (2)0.022 (2)0.0077 (17)−0.0013 (16)−0.0004 (15)
C240.023 (2)0.015 (2)0.0157 (18)0.0065 (17)0.0001 (15)0.0016 (14)
C250.038 (3)0.028 (2)0.0140 (19)0.007 (2)−0.0021 (17)−0.0022 (16)
C260.046 (3)0.026 (2)0.018 (2)0.013 (2)0.0090 (19)0.0028 (17)
C270.031 (2)0.021 (2)0.021 (2)0.0073 (19)0.0110 (17)0.0046 (16)
C280.023 (2)0.017 (2)0.0181 (19)0.0040 (18)0.0033 (15)0.0017 (15)
W1—C22.142 (4)N6—C61.153 (5)
W1—C42.144 (4)N7—C71.160 (5)
W1—C32.149 (4)N8—C81.157 (5)
W1—C12.150 (4)N9—C91.343 (5)
W1—C72.159 (4)N9—C131.356 (5)
W1—C82.170 (4)N10—C181.346 (5)
W1—C62.186 (4)N10—C141.351 (5)
W1—C52.187 (4)N11—C191.333 (5)
Mn1—N2i2.151 (3)N11—C231.351 (5)
Mn1—N12.176 (3)N12—C281.342 (5)
Mn1—O22.221 (3)N12—C241.349 (5)
Mn1—N102.234 (3)C9—C101.391 (5)
Mn1—O12.244 (3)C9—H90.9500
Mn1—N92.254 (3)C10—C111.382 (6)
Mn2—N32.150 (3)C10—H100.9500
Mn2—N4ii2.201 (3)C11—C121.395 (6)
Mn2—O42.219 (3)C11—H110.9500
Mn2—O32.229 (3)C12—C131.378 (5)
Mn2—N122.248 (3)C12—H120.9500
Mn2—N112.249 (3)C13—C141.493 (5)
O1—H10.836 (19)C14—C151.398 (5)
O1—H20.842 (19)C15—C161.388 (6)
O2—H30.834 (19)C15—H150.9500
O2—H40.822 (19)C16—C171.384 (6)
O3—H50.824 (19)C16—H160.9500
O3—H60.829 (19)C17—C181.381 (5)
O4—H70.837 (19)C17—H170.9500
O4—H80.830 (19)C18—H180.9500
O5—H290.835 (19)C19—C201.385 (6)
O5—H300.836 (19)C19—H190.9500
O6—H310.833 (19)C20—C211.383 (6)
O6—H320.827 (19)C20—H200.9500
O7—H330.826 (19)C21—C221.374 (7)
O7—H340.824 (19)C21—H210.9500
O8—H360.831 (19)C22—C231.396 (5)
O8—H350.828 (19)C22—H220.9500
O9—H370.834 (19)C23—C241.492 (6)
O9—H380.839 (19)C24—C251.394 (5)
N1—C11.163 (5)C25—C261.378 (7)
N2—C21.158 (5)C25—H250.9500
N2—Mn1ii2.151 (3)C26—C271.391 (6)
N3—C31.154 (5)C26—H260.9500
N4—C41.153 (5)C27—C281.384 (5)
N4—Mn2i2.201 (3)C27—H270.9500
N5—C51.146 (5)C28—H280.9500
C2—W1—C4107.63 (14)C9—N9—Mn1124.7 (2)
C2—W1—C376.34 (14)C13—N9—Mn1116.6 (2)
C4—W1—C3142.60 (13)C18—N10—C14118.8 (3)
C2—W1—C1142.96 (14)C18—N10—Mn1123.8 (3)
C4—W1—C184.20 (13)C14—N10—Mn1117.3 (2)
C3—W1—C173.85 (14)C19—N11—C23119.1 (3)
C2—W1—C784.55 (15)C19—N11—Mn2124.2 (3)
C4—W1—C7145.08 (14)C23—N11—Mn2116.7 (3)
C3—W1—C771.42 (14)C28—N12—C24118.5 (3)
C1—W1—C7105.89 (14)C28—N12—Mn2124.1 (2)
C2—W1—C873.08 (15)C24—N12—Mn2117.4 (3)
C4—W1—C871.85 (14)N1—C1—W1178.5 (3)
C3—W1—C874.17 (14)N2—C2—W1177.7 (3)
C1—W1—C878.01 (14)N3—C3—W1178.6 (3)
C7—W1—C8142.45 (15)N4—C4—W1175.6 (3)
C2—W1—C670.17 (14)N5—C5—W1176.7 (3)
C4—W1—C675.29 (14)N6—C6—W1177.0 (3)
C3—W1—C6136.71 (14)N7—C7—W1178.2 (4)
C1—W1—C6146.11 (14)N8—C8—W1178.8 (4)
C7—W1—C678.73 (14)N9—C9—C10123.1 (4)
C8—W1—C6119.10 (14)N9—C9—H9118.4
C2—W1—C5143.73 (14)C10—C9—H9118.4
C4—W1—C575.60 (13)C11—C10—C9117.9 (4)
C3—W1—C5123.59 (13)C11—C10—H10121.1
C1—W1—C572.70 (14)C9—C10—H10121.1
C7—W1—C575.84 (14)C10—C11—C12119.6 (4)
C8—W1—C5137.85 (14)C10—C11—H11120.2
C6—W1—C576.19 (13)C12—C11—H11120.2
N2i—Mn1—N196.57 (13)C13—C12—C11119.2 (4)
N2i—Mn1—O282.20 (12)C13—C12—H12120.4
N1—Mn1—O2169.50 (12)C11—C12—H12120.4
N2i—Mn1—N1093.95 (12)N9—C13—C12121.7 (4)
N1—Mn1—N1089.84 (12)N9—C13—C14116.0 (3)
O2—Mn1—N10100.64 (12)C12—C13—C14122.3 (3)
N2i—Mn1—O192.57 (12)N10—C14—C15121.4 (4)
N1—Mn1—O181.90 (12)N10—C14—C13116.4 (3)
O2—Mn1—O187.73 (12)C15—C14—C13122.2 (4)
N10—Mn1—O1170.02 (12)C16—C15—C14119.0 (4)
N2i—Mn1—N9159.83 (12)C16—C15—H15120.5
N1—Mn1—N999.14 (12)C14—C15—H15120.5
O2—Mn1—N984.59 (11)C17—C16—C15119.4 (4)
N10—Mn1—N973.59 (11)C17—C16—H16120.3
O1—Mn1—N9102.08 (11)C15—C16—H16120.3
N3—Mn2—N4ii92.55 (12)C18—C17—C16118.7 (4)
N3—Mn2—O483.38 (12)C18—C17—H17120.6
N4ii—Mn2—O4165.86 (11)C16—C17—H17120.6
N3—Mn2—O3100.21 (12)N10—C18—C17122.7 (4)
N4ii—Mn2—O383.18 (11)N10—C18—H18118.7
O4—Mn2—O384.22 (11)C17—C18—H18118.7
N3—Mn2—N1293.06 (12)N11—C19—C20122.9 (4)
N4ii—Mn2—N1291.00 (11)N11—C19—H19118.6
O4—Mn2—N12102.71 (11)C20—C19—H19118.6
O3—Mn2—N12165.71 (12)C21—C20—C19118.4 (4)
N3—Mn2—N11162.59 (12)C21—C20—H20120.8
N4ii—Mn2—N1198.25 (12)C19—C20—H20120.8
O4—Mn2—N1189.14 (11)C22—C21—C20119.3 (4)
O3—Mn2—N1194.61 (12)C22—C21—H21120.4
N12—Mn2—N1173.24 (12)C20—C21—H21120.4
Mn1—O1—H1109 (3)C21—C22—C23119.6 (4)
Mn1—O1—H2110 (3)C21—C22—H22120.2
H1—O1—H2106 (5)C23—C22—H22120.2
Mn1—O2—H3133 (3)N11—C23—C22120.8 (4)
Mn1—O2—H4121 (3)N11—C23—C24116.5 (3)
H3—O2—H4106 (5)C22—C23—C24122.6 (4)
Mn2—O3—H5110 (3)N12—C24—C25121.7 (4)
Mn2—O3—H6118 (3)N12—C24—C23115.8 (3)
H5—O3—H6105 (5)C25—C24—C23122.5 (4)
Mn2—O4—H7120 (3)C26—C25—C24119.0 (4)
Mn2—O4—H8114 (3)C26—C25—H25120.5
H7—O4—H8104 (4)C24—C25—H25120.5
H29—O5—H30107 (5)C25—C26—C27119.7 (4)
H31—O6—H32114 (4)C25—C26—H26120.1
H33—O7—H34104 (5)C27—C26—H26120.1
H36—O8—H35114 (5)C28—C27—C26117.9 (4)
H37—O9—H38111 (5)C28—C27—H27121.0
C1—N1—Mn1158.7 (3)C26—C27—H27121.0
C2—N2—Mn1ii159.8 (3)N12—C28—C27123.2 (4)
C3—N3—Mn2176.1 (3)N12—C28—H28118.4
C4—N4—Mn2i146.4 (3)C27—C28—H28118.4
C9—N9—C13118.4 (3)
N2i—Mn1—N1—C1−7.6 (8)C5—W1—C4—N4−25 (4)
O2—Mn1—N1—C1−90.2 (11)C2—W1—C5—N5−95 (6)
N10—Mn1—N1—C186.4 (8)C4—W1—C5—N55(6)
O1—Mn1—N1—C1−99.3 (8)C3—W1—C5—N5149 (6)
N9—Mn1—N1—C1159.7 (8)C1—W1—C5—N593 (6)
N4ii—Mn2—N3—C3−3(4)C7—W1—C5—N5−155 (6)
O4—Mn2—N3—C3163 (4)C8—W1—C5—N545 (6)
O3—Mn2—N3—C380 (4)C6—W1—C5—N5−73 (6)
N12—Mn2—N3—C3−94 (4)C2—W1—C6—N619 (6)
N11—Mn2—N3—C3−132 (4)C4—W1—C6—N6135 (6)
N2i—Mn1—N9—C9−128.7 (4)C3—W1—C6—N6−22 (7)
N1—Mn1—N9—C990.6 (3)C1—W1—C6—N6−171 (6)
O2—Mn1—N9—C9−79.5 (3)C7—W1—C6—N6−69 (6)
N10—Mn1—N9—C9177.7 (3)C8—W1—C6—N676 (6)
O1—Mn1—N9—C97.0 (3)C5—W1—C6—N6−147 (6)
N2i—Mn1—N9—C1357.1 (5)C2—W1—C7—N7−20 (12)
N1—Mn1—N9—C13−83.6 (3)C4—W1—C7—N794 (12)
O2—Mn1—N9—C13106.3 (3)C3—W1—C7—N7−97 (12)
N10—Mn1—N9—C133.6 (3)C1—W1—C7—N7−163 (12)
O1—Mn1—N9—C13−167.2 (3)C8—W1—C7—N7−72 (12)
N2i—Mn1—N10—C1817.3 (3)C6—W1—C7—N751 (12)
N1—Mn1—N10—C18−79.3 (3)C5—W1—C7—N7130 (12)
O2—Mn1—N10—C18100.1 (3)C2—W1—C8—N8−11 (18)
O1—Mn1—N10—C18−113.3 (7)C4—W1—C8—N8−127 (18)
N9—Mn1—N10—C18−178.8 (3)C3—W1—C8—N869 (18)
N2i—Mn1—N10—C14−166.1 (3)C1—W1—C8—N8145 (18)
N1—Mn1—N10—C1497.3 (3)C7—W1—C8—N845 (18)
O2—Mn1—N10—C14−83.3 (3)C6—W1—C8—N8−66 (18)
O1—Mn1—N10—C1463.3 (8)C5—W1—C8—N8−168 (18)
N9—Mn1—N10—C14−2.2 (3)C13—N9—C9—C102.8 (6)
N3—Mn2—N11—C19−142.6 (4)Mn1—N9—C9—C10−171.3 (3)
N4ii—Mn2—N11—C1989.6 (3)N9—C9—C10—C11−2.4 (6)
O4—Mn2—N11—C19−78.3 (3)C9—C10—C11—C12−0.6 (6)
O3—Mn2—N11—C195.8 (3)C10—C11—C12—C133.0 (6)
N12—Mn2—N11—C19178.1 (4)C9—N9—C13—C12−0.2 (6)
N3—Mn2—N11—C2333.3 (6)Mn1—N9—C13—C12174.4 (3)
N4ii—Mn2—N11—C23−94.5 (3)C9—N9—C13—C14−178.9 (3)
O4—Mn2—N11—C2397.6 (3)Mn1—N9—C13—C14−4.3 (4)
O3—Mn2—N11—C23−178.2 (3)C11—C12—C13—N9−2.7 (6)
N12—Mn2—N11—C23−5.9 (3)C11—C12—C13—C14176.0 (4)
N3—Mn2—N12—C2816.4 (3)C18—N10—C14—C15−0.3 (5)
N4ii—Mn2—N12—C28−76.2 (3)Mn1—N10—C14—C15−177.1 (3)
O4—Mn2—N12—C28100.3 (3)C18—N10—C14—C13177.6 (3)
O3—Mn2—N12—C28−141.9 (4)Mn1—N10—C14—C130.8 (4)
N11—Mn2—N12—C28−174.5 (3)N9—C13—C14—N102.4 (5)
N3—Mn2—N12—C24−165.9 (3)C12—C13—C14—N10−176.4 (4)
N4ii—Mn2—N12—C24101.5 (3)N9—C13—C14—C15−179.8 (3)
O4—Mn2—N12—C24−82.0 (3)C12—C13—C14—C151.5 (6)
O3—Mn2—N12—C2435.8 (6)N10—C14—C15—C160.6 (6)
N11—Mn2—N12—C243.2 (3)C13—C14—C15—C16−177.2 (4)
Mn1—N1—C1—W1127 (14)C14—C15—C16—C170.0 (6)
C2—W1—C1—N119 (14)C15—C16—C17—C18−0.7 (6)
C4—W1—C1—N1−93 (14)C14—N10—C18—C17−0.5 (6)
C3—W1—C1—N156 (14)Mn1—N10—C18—C17176.1 (3)
C7—W1—C1—N1121 (14)C16—C17—C18—N101.0 (6)
C8—W1—C1—N1−20 (14)C23—N11—C19—C20−0.6 (6)
C6—W1—C1—N1−145 (14)Mn2—N11—C19—C20175.2 (3)
C5—W1—C1—N1−170 (100)N11—C19—C20—C21−0.2 (7)
Mn1ii—N2—C2—W19(10)C19—C20—C21—C220.2 (7)
C4—W1—C2—N2−77 (9)C20—C21—C22—C230.6 (7)
C3—W1—C2—N2141 (9)C19—N11—C23—C221.4 (6)
C1—W1—C2—N2179 (100)Mn2—N11—C23—C22−174.7 (3)
C7—W1—C2—N269 (9)C19—N11—C23—C24−176.1 (4)
C8—W1—C2—N2−141 (9)Mn2—N11—C23—C247.8 (4)
C6—W1—C2—N2−11 (9)C21—C22—C23—N11−1.4 (6)
C5—W1—C2—N212 (9)C21—C22—C23—C24175.9 (4)
Mn2—N3—C3—W1−10 (18)C28—N12—C24—C25−0.5 (6)
C2—W1—C3—N3−4(14)Mn2—N12—C24—C25−178.3 (3)
C4—W1—C3—N3−106 (14)C28—N12—C24—C23177.5 (3)
C1—W1—C3—N3−162 (14)Mn2—N12—C24—C23−0.4 (4)
C7—W1—C3—N384 (14)N11—C23—C24—N12−4.9 (5)
C8—W1—C3—N3−80 (14)C22—C23—C24—N12177.7 (4)
C6—W1—C3—N335 (14)N11—C23—C24—C25173.0 (4)
C5—W1—C3—N3142 (14)C22—C23—C24—C25−4.4 (6)
Mn2i—N4—C4—W1−21 (5)N12—C24—C25—C260.5 (6)
C2—W1—C4—N4118 (4)C23—C24—C25—C26−177.3 (4)
C3—W1—C4—N4−152 (4)C24—C25—C26—C270.1 (6)
C1—W1—C4—N4−98 (4)C25—C26—C27—C28−0.7 (6)
C7—W1—C4—N411 (4)C24—N12—C28—C27−0.2 (6)
C8—W1—C4—N4−178 (4)Mn2—N12—C28—C27177.6 (3)
C6—W1—C4—N454 (4)C26—C27—C28—N120.7 (6)
D—H···AD—HH···AD···AD—H···A
O1—H1···O10i0.84 (2)2.02 (2)2.822 (5)162 (5)
O1—H2···O9iii0.84 (2)2.04 (3)2.834 (4)156 (5)
O2—H3···O6iv0.83 (2)1.87 (2)2.703 (4)173 (5)
O2—H4···N6i0.82 (2)2.25 (2)3.052 (4)165 (5)
O3—H6···O6ii0.83 (2)1.92 (2)2.744 (4)176 (5)
O3—H5···N5ii0.82 (2)2.48 (3)3.238 (4)153 (4)
O4—H8···O5ii0.83 (2)2.12 (2)2.907 (5)159 (4)
O4—H7···O9v0.84 (2)1.89 (2)2.722 (4)174 (4)
O5—H30···N6vi0.84 (2)2.13 (2)2.946 (5)164 (5)
O5—H29···O1i0.84 (2)2.32 (3)3.111 (4)157 (5)
O6—H32···O70.83 (2)1.97 (2)2.773 (4)162 (5)
O6—H31···O50.83 (2)1.97 (3)2.753 (4)157 (4)
O7—H34···N8i0.82 (2)2.02 (2)2.810 (5)159 (4)
O7—H33···N50.83 (2)2.09 (2)2.915 (5)175 (4)
O8—H35···N7vii0.83 (2)2.03 (2)2.840 (5)165 (5)
O8—H36···O70.83 (2)2.03 (2)2.854 (4)174 (5)
O9—H38···N6vii0.84 (2)2.66 (3)3.372 (5)143 (4)
O9—H37···O80.83 (2)1.91 (2)2.715 (5)161 (5)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1—H1⋯O10i0.84 (2)2.02 (2)2.822 (5)162 (5)
O1—H2⋯O9ii0.84 (2)2.04 (3)2.834 (4)156 (5)
O2—H3⋯O6iii0.83 (2)1.87 (2)2.703 (4)173 (5)
O2—H4⋯N6i0.82 (2)2.25 (2)3.052 (4)165 (5)
O3—H6⋯O6iv0.83 (2)1.92 (2)2.744 (4)176 (5)
O3—H5⋯N5iv0.82 (2)2.48 (3)3.238 (4)153 (4)
O4—H8⋯O5iv0.83 (2)2.12 (2)2.907 (5)159 (4)
O4—H7⋯O9v0.84 (2)1.89 (2)2.722 (4)174 (4)
O5—H30⋯N6vi0.84 (2)2.13 (2)2.946 (5)164 (5)
O5—H29⋯O1i0.84 (2)2.32 (3)3.111 (4)157 (5)
O6—H32⋯O70.83 (2)1.97 (2)2.773 (4)162 (5)
O6—H31⋯O50.83 (2)1.97 (3)2.753 (4)157 (4)
O7—H34⋯N8i0.82 (2)2.02 (2)2.810 (5)159 (4)
O7—H33⋯N50.83 (2)2.09 (2)2.915 (5)175 (4)
O8—H35⋯N7vii0.83 (2)2.03 (2)2.840 (5)165 (5)
O8—H36⋯O70.83 (2)2.03 (2)2.854 (4)174 (5)
O9—H38⋯N6vii0.84 (2)2.66 (3)3.372 (5)143 (4)
O9—H37⋯O80.83 (2)1.91 (2)2.715 (5)161 (5)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) .

  3 in total

1.  X-ray evidence of CN bridging in bimetallic complexes based on [M(CN)8]4- (M = Mo, W). The crystal structure of [[Mn(bpy)2]2(mu-NC)2[Mo(CN)6]2(mu-CN)2[Mn(bpy)2]2].8H2O.

Authors:  B Sieklucka; J Szklarzewicz; T J Kemp; W Errington
Journal:  Inorg Chem       Date:  2000-10-30       Impact factor: 5.165

2.  Synthesis and alcohol vapor sensitivity of a ferromagnetic copper-tungsten bimetallic assembly.

Authors:  Shin-ichi Ohkoshi; Yoshihide Tsunobuchi; Hitomi Takahashi; Toshiya Hozumi; Motoo Shiro; Kazuhito Hashimoto
Journal:  J Am Chem Soc       Date:  2007-02-21       Impact factor: 15.419

3.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290
  3 in total

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