Supporting Information for Inorg. Chem., 1994, 33(7), , DOI: /ic00085a003 OHTO
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1 Supporting Information for Inorg. Chem., 1994, 33(7), , DOI: /ic00085a003 OHTO Terms& Conditions Electronic Supporting Information files are available without a subscription to ACS Web Editions. The American Chemical Society holds a copyright ownership interest in any copyrightable Supporting Information. Files available from the ACS website may be downloaded for personal use only. Users are not otherwise permitted to reproduce, republish, redistribute, or sell any Supporting Information from the ACS website, either in whole or in part, in either machine-readable form or any other form without permission from the American Chemical Society. For permission to reproduce, republish and redistribute this material, requesters must process their own requests via the RightsLink permission system. Information about how to use the RightsLink permission system can be found at Copyright 1994 American Chemical Society
2 Table SI, X-ray Crystallographic Details for [Ru2Co(/.i3-O)0u-CH3COO)6(py)3]*py A. Crystal Data J o / ' " / T j/ Empirical Formula Formula Weight Crystal Color, Habit Crystal System Lattice Type No. of Reflections Used for Unit Cell Determination (26 range) Lattice Parameters Space Group Z value ^calc FOOO /i(moka) R U 2 C 0 C 3 2 H 3 8 N 4 O black, prismatic trigonal R-centered 20( ) a = (5) A 0 = (6) A V = 2949(1) A3 R32 (#155) g/cm cm-1 B. Intensity Measurements Diffractometer Radiation Temperature Scan Type Scan Rate Scan Width 2$max No. of Reflections Measured Corrections Rigaku AFC-5R MoKot (K =0,71069 A) graphite monochromated room temperature O) 4.0 /min (in co) ( tan 0) 55.2 Total: 4727 Unique; 832 (Rint = 0.047) Lorentz-polarization C. Structure Solution and Refinement Stincture Solution Refinement Function Minimized Least Squares Weights Anomalous Dispersion No. Observations (I>3.00cf(I)) No. Variables Reflection/Parameter Ratio Residuals: R; Rw Goodness of Fit Indicator Max Shift/Error in Final Cycle Maximum peak in Final Diff. Map Minimum peak in Final Diff. Map Direct Methods Full-matrix least-squares CO(IFol - IFcl)2 l/o 2(Fo) = 4Fo2/<j2(Fo2) All non-hydrogen atoms ; e'/a e /A3 (S2)
3 Table S2. Atomic Coordinates and BjS0/B Cq for [Ru2 Co(/i3 -D)(/x-CH3COO)6 (py)3] *py atom X y z ^iso^eq M (3) (10) 0(1) (8) 0(2) (3) (3) (3} 4.81(9) 0(3) (2) (3) (3) 4.85(9) N(l) (3) (1) C(l) (4) (3) (4) 4.0(1) C(2) (5) (5) (6) 7.4(2) C(3) (4) (4) (5) 4.8(1) C(4) (5) (5) (6) 5.9(2) C(5) (5) (2) C(6)t (3) 12.7(8)t C(7)t 0.026(3) 0.076(3) 0.463(2) 12(l)t- C(B)t (2) (2) 0.399(3) 6.8(6)*+ Beq = 8rc^(C/ii(aa*)2+C/22(bb!,<)^+C/33(cc*)^+2t/i2 aa*bb*cosy+2l/i3 aa*cc*cosp+2[/23 bb*cc*cosa) / 3 f solvate pyridine ring atom. Because of the disorder of the solvate pyridine molecule(see text), the structure has been solved assuming that pyridine nitrogen is carbon atom. B[so Table S3. Anisotropic Displacement Parameters for [Ru2Co(/i3-0)(^-CH3COQ)6(py)3] py atom u n U22 ^33 ^12 ^13 U23 M (2) (3) (2) (1) (1) 0.027(2) (4) (2) 0.055(2) 0.066(2) 0.076(2) 0.041(2) 0.024(2) 0.024(2) 0(3) 0.045(2) 0.065(2) 0.085(2) 0.035(2) (2) (2) N(l) 0.035(2) 0.047(3) 0.054(3) (1) C(l) 0.044(3) 0.045(3) 0.063(3) 0.021(2) 0.018(2) 0.012(2) C(2) 0.090(5) 0.084(5) 0.117(5) 0.051(4) 0.074(5) 0.050(4) C(3) 0.055(3) 0.055(3) 0.090(3) 0.040(3) (3) (2) C(4) 0.066(4) 0.083(4) 0.102(4) 0.057(4) (3) (3) C(5) 0.052(4) 0.096(8) 0.117(7) (3) The general temperature factor expression: exp(-27r2(a*2c/iih2+b*2t/22k2+c*2t/33i2+2a*b*t/i2hk+2a;t;c*t/]3hl++2b:ficifst/23k0) (S3)
4 Table S4. Intermolecular Atomic Bond Distances for [Ru2Co(/.i3-O)0u-CH3COO)6(py)3]*py atom atom distance(a) M M 3.359(1) M 0(1) (8) M 0(2) 2.053(3) M 0(3) 2.070(3) M N(l) 2.174(5) 0(2) C(l) 1.247(6) 0(3) C(1) 1.234(6) N(l) 0(3) 1.326(6) C(l) 0(2) 1.526(7) C(3) 0(4) 1.400(9) C(4) 0(5) 1.395(8) Table S5. Intermolecular Bond Angles for [Ru2C0 (^3-O)(/i-CIi3COO)6(py)3]*py atom atom atom angle(deg.) M 0(1) M M 0(2) 0(1) 130.7(4) M N(l) 0(3) 120.4(4) 0(1) M 0(2) 94.8(1) 0(1) M 0(3) 94.8(1) 0(1) M N(l) (2) M 0(3) 90.0(2) 0(2) M N(l) 85.2(1) 0(3) M N (l) 85.2(1) 0(2) C(l) 0(3)' 126.9(5) 0(2) 0(1) C(2) 116.1(5) 0(2) 0(1) 0(3)' 116.9(5) 0(3) 0(4) 0(5) 116.8(7) N(l) 0(3) 0(4) 123.2(6) (S4)
5 Table S6. X-ray Crystallographic Details for [Ru2Ni(/.i3-0)(/z-CH3C00)6(py)3]#py A. Crystal Data Empirical Formula Formula Weight Crystal Color, Habit Crystal System Lattice Type No. of Reflections Used for Unit Cell Determination (20 range) Lattice Parameters Space Group Z value ^catc Fooo /i(mokot) Ru2NiC32H3sN40i black, prismatic trigonal R-centered 20( ) a = (4) A c = (5) A V = 2935(1) A3 V?32(#l 55) 3 1,61 g/cm cm-1 B. Intensity Measurements Diffractometer Radiation Temperature Scan Type Scan Rate Scan Width 2^max No. of Reflections Measured Corrections Rigaku AFC-5R M ok a (X = A) graphite monochromated room temperature co /min (in co) ( tan(9) 55.3 Total: 4734 Unique: 834 (RinL = 0.039) Lorentz-polarization C. Structure Solution and Refinement Structure Solution Refinement Function Minimized. Least Squares Weights Anomalous Dispersion No. Observations (I>3.00c(I)) No. Variables Reflection/Parameter Ratio Residuals: R; Rw Goodness of Fit Indicator Max Shift/Error in Final Cycle Maximum peak in Final Diff. Map Minimum peak in Final Diff. Map Direct Methods Full-matrix least-squares S co (IFol - IFcl)2 l/a 2(Fo) = 4F o2/o2(fo2) All non-hydrogen atoms ; e'/a e'/a3 (S5)
6 atom X y z ^iso^eq M (3) (1) 0(1) (9) 0(2) (3) (3) (4) 4.8(1) 0(3) (3) (3) (4) 4.71(10) N(l) (4) (1) C(l) (4) (4) (5) 3.9(1) C(2) (6) (6) (7) 7.2(2) C(3) (5) (4) (6) 4.5(1) C(4) (5) (6) (8) 5.7(2) C(5) (6) (3) C(6)t (2) 11.2(6)+ C(7)t 0.029(6) 0.084(4) 0.439(4) 12(1)* C(8)t 0.058(2) (2) 0.413(3) 14.1(6)* Beq = 8n:2(C/n(aa*)2+i[/22(bb*)2+(733(cc!i<)2+20ri2 aa*bb*cosy+2 /i3 aa*cc*cosp+2c/23 bb*cc*cosa) / 3 t solvate pyridine ring atom, Because of the disorder of tlie solvate pyridine molecule(see text), the structure has been solved assuming that pyridine nitrogen is carbon atom. $ B l50 Table S8. Anisotropic Displacement Parameters for [Ru2Ni(/.i3-0)( i-ch.3c00)6(py)3]*py atom UU: U22 ^33 Ul3 ^23 M (2) (3) (3) (1) (1) 0.032(3) (5) (2) 0.051(3) 0.065(3) 0.081(3) 0.039(2) 0.024(2) 0.025(2) 0(3) 0.048(2) 0.063(3) 0.081(3) 0.037(2) (2) (2) N(l) 0.036(2) 0.042(3) 0.050(4) (1) C(l) 0.042(3) 0.043(3) 0.059(3) 0.019(3) 0.014(2) 0.009(3) C(2) 0.096(6) 0.088(6) 0.110(5) 0.061(5) 0.068(5) 0.054(5) C(3) 0.055(3) 0.047(3) 0.085(4) 0.037(3) (4) (3) C(4) 0.063(4) 0.072(5) 0.101(6) 0.049(4) (4) (4) C(5) 0.055(4) 0.110(9) 0.093(8) (4) The general temperature factor expression: exp(-27i:2(a*2( /n h 2+b*2t/22k2+c*2C/33l2+2a*b*t/ i2hk+2a*c;,''t/i3hl++2b*c*t/23kl)) (S6)
7 Table S9. Interm olecular Atomic Bond Distances for [Ru2Ni((U3-0)(/i-CH3C00)6(py)3]*py atom. atom distance(a) M M 3.346(1) M 0(1) (7) U 0(2) 2.052(4) M 0(3) 2.057(4) M N(l) 2.136(6) 0(2) c(n 1.249(8) 0 (3 ) C(1) 1.237(7) N(l) 0(3) 1.334(7) C(l) 0(2) 1.519(9) C(3) 0(4) 1.39(1) 0(4) 0(5) 1.375(10) Table SIO. Intermolecular Bond Angles for [Ru2Ni(/i3-0)(/i-CH3C00)6(py)3]*py atom atom atom angle(deg.) M 0(1) M M 0(2) 0(1) 130.6(4) M N(l) 0(3) 121.3(4) 0(1) M 0(3) 94.8(1) 0(1) M N(l) (1) M 0(2) 95.0(1) 0(2) M 0(3) 90.3(2) 0(2) M N(l) 85.0(1) 0(3) M N(l) 85.2(1) 0(2) 0(1) C(2) 115.8(6) 0(2) 0(1) 0(3)' 126.4(6) 0(2) 0(1) 0(3 ) 117.8(6) 0(3) 0(4) 0(5) 117.1(8) N(l) 0(3) 0(4) 123.5(7) (S7)
8 Labeling Scheme for rr!;2co( /3-0)(i/-CH3C()0)6(py)3j-py
9 Labeling Scheme for [Ru2Ni(/i.3-0)(iu-CH3C00)6(py)3]*py
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