mirela-fernanda zaltariov, maria cazacu, sergiu shova, cristian … · 2015-12-04 · supplementary...
TRANSCRIPT
Supplementary data
A silicon-containing polyazomethine and derived metal complexes: synthesis, characterization
and evaluation of the properties
Mirela-Fernanda Zaltariov, Maria Cazacu, Sergiu Shova, Cristian Varganici, Loredana
Vacareanu, Valentina Musteata, Anton Airinei
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Figure 1S. FTIR spectrum of 2,5-bis(p-aminophenyl)-1,3,4-oxadiazole.
Supplemental
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Figure 2S. 1H NMR Spectrum for 2,5-bis(p-aminophenyl)-1,3,4-oxadiazole.
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Figure 3S.
13C NMR Spectrum for 2,5-bis(p-aminophenyl)-1,3,4-oxadiazole.
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Figure 4S. FT-IR Spectrum for bis(formyl-p-phenoxymethyl)-dimethylsilane, DA.
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Figure 5S. 1H NMR Spectrum for bis(formyl-p-phenoxymethyl)-dimethylsilane, DA.
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Fig. 6S 13
C NMR Spectrum for bis(formyl-p-phenoxymethyl)-dimethylsilane, DA
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Figure 7S. FTIR spectrum of polyazomethine PAZ.
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Figure 8S. 1HNMR spectrum for polyazomethine PAZ.
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Figure 9S. FTIR spectrum of Cu complex, PAZ-Cu.
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Figure 10S. FTIR spectrum of Co complex, PAZ-Co.
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Figure 11S. FTIR spectrum of Zn complex, PAZ-Zn.
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Figure 12S. Comparative IR spectra details for polyazomethine and metal complexes
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Figure 13S. Far-IR spectrum of Cu complex, PAZ-Cu.
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Figure 14S. Far-IR spectrum of Co complex, PAZ-Co.
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Figure 15S. Far-IR spectrum of Zn complex, PAZ-Zn.
Figure 16S. DTG curves of the polyazomethine-based structures
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Figure 17S. PAZ-Co: (a) cyclic voltammogram recorded during the potential electrode scanning
from 0.0 V to 1.5 V range with 50 mV/s; (b) cyclic voltammogram recorded during the electrode
potential scanning from +1.5 V to -1.5 V range with 50 mV/s; (c) the multi cyclic voltammograms
(10 cycles) recorded for PAZ-Co on the positive range of potential; (d) cyclic voltammograms of
PAZ-Co recorded at different scan rates (from 20 to 250 mV/s).
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Figure 18S. PAZ-Zn: (a) cyclic voltammogram recorded during the potential electrode scanning
from 0.0 V to 1.4 V range with 50 mV/s; (b) cyclic voltammogram recorded during the electrode
potential scanning from +1.4 V to -1.4 V range with 50 mV/s; (c) the multi cyclic voltammograms
(10 cycles) recorded for PAZ-Zn on the positive range of potential; (d) cyclic voltammograms of
PAZ-Zn recorded at different scan rates (from 20 to 250 mV/s).
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Figure 19S. Temperature dependence of the ac conductivity ac, dielectric permittivity ` and
dielectric loss `` of PAZ-Co at different frequencies (in Hz).
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Figure 20S. Temperature dependence of the ac conductivity ac, dielectric permittivity ` and
dielectric loss `` of PAZ-Zn at different frequencies (in Hz).
checkCIF/PLATON report
No syntax errors found. CIF dictionary Interpreting this report
Datablock: shi_1786_mz
Bond precision: C-C = 0.0044 A Wavelength=0.71070
Cell: a=10.2109(6) b=19.6215(8) c=9.5424(4)alpha=90 beta=110.916(6) gamma=90
Temperature: 299 K
Calculated ReportedVolume 1785.87(16) 1785.87(15)Space group C c C 1 c 1 Hall group C -2yc C -2yc Moiety formula C18 H20 O4 Si C18 H20 O4 SiSum formula C18 H20 O4 Si C18 H20 O4 SiMr 328.43 328.43Dx,g cm-3 1.222 1.222Z 4 4Mu (mm-1) 0.148 0.148F000 696.0 696.0F000’ 696.65h,k,lmax 12,24,11 12,24,11Nref 1758[ 3504] 3255 Tmin,Tmax 0.957,0.985 0.861,1.000Tmin’ 0.936
Correction method= MULTI-SCAN
Data completeness= 1.85/0.93 Theta(max)= 26.000
R(reflections)= 0.0465( 2696) wR2(reflections)= 0.1177( 3255)
S = 1.031 Npar= 210
The following ALERTS were generated. Each ALERT has the format test-name_ALERT_alert-type_alert-level .Click on the hyperlinks for more details of the test.
Alert level B Crystal system given = monoclinicPLAT018_ALERT_1_B _diffrn_measured_fraction_theta_max .NE. _full !
Alert level CPLAT230_ALERT_2_C Hirshfeld Test Diff for Si1 -- C9 .. 6.0 su
Compound 1_cifreport
PLAT230_ALERT_2_C Hirshfeld Test Diff for Si1 -- C10 .. 5.5 su PLAT230_ALERT_2_C Hirshfeld Test Diff for Si1 -- C11 .. 6.5 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Si1 PLAT340_ALERT_3_C Low Bond Precision on C-C Bonds ............... 0.0044 Ang
Alert level GPLAT005_ALERT_5_G No _iucr_refine_instructions_details in the CIF ?PLAT093_ALERT_1_G No su’s on H-positions, refinement reported as . mixed
0 ALERT level A = Most likely a serious problem - resolve or explain 1 ALERT level B = A potentially serious problem, consider carefully 5 ALERT level C = Check. Ensure it is not caused by an omission or oversight 2 ALERT level G = General information/check it is not something unexpected
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
It is advisable to attempt to resolve as many as possible of the alerts in all categories. Oftenthe minor alerts point to easily fixed oversights, errors and omissions in your CIF orrefinement strategy, so attention to these fine details can be worthwhile. In order to resolvesome of the more serious problems it may be necessary to carry out additional measurementsor structure refinements. However, the purpose of your study may justify the reporteddeviations and the more serious of these should normally be commented upon in thediscussion or experimental section of a paper or in the "special_details" fields of the CIF.checkCIF was carefully designed to identify outliers and unusual parameters, but every testhas its limitations and alerts that are not important in a particular case may appear.Conversely, the absence of alerts does not guarantee there are no aspects of the resultsneeding attention. It is up to the individual to critically assess their own results and, ifnecessary, seek expert advice.
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PLATON version of 05/11/2012; check.def file version of 05/11/2012
Datablock shi_1786_mz - ellipsoid plot