June 22, 2012 67 th Symp. on Molec. Spectrosc. Laboratory Detection of ClZnCH 3 (X 1 A 1 ): Further Evidence for Zinc Insertion Matthew P. Bucchino and.

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June 22, th Symp. on Molec. Spectrosc. Laboratory Detection of ClZnCH 3 (X 1 A 1 ): Further Evidence for Zinc Insertion Matthew P. Bucchino and Lucy M. Ziurys Department of Chemistry Steward Observatory University of Arizona 97 th Canadian Chemistry Conference and Exhibition June 3, th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. 69 th Symp. on Molec. Spectrosc. June 18, 2014 More Negishi!!!

June 22, th Symp. on Molec. Spectrosc. Previous Work: ClZnCH 3 M + CH 4 → CH 3 –M–H (M = Pd, Be, Mg, Ca, Zn, Cd) M + CH 3 Cl → CH 3 –M–Cl (M = Pd, Mg, Zn, Cd) 69 th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. Instrumentation -Phase-locked Gunn oscillators and Schottky diode multipliers ( GHz) -Gaussian beam optics -Reaction chamber: double-pass stainless steel cell -InSb He-cooled bolometer -Phase sensitive detection (2f) Broida Oven Direct Absorption Spectrometer 68 th Symp. on Molec. Spectrosc. June 19, th Canadian Chemistry Conference and Exhibition June 3, th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. ClZnCH 3 Synthesis –Broida-type Oven → Zn vapor – mTorr CH 3 Cl from top –15 mTorr Ar from bottom/side –0.050 A (300 V) DC discharge IZnCH 3 Synthesis –Broida-type Oven → Zn vapor –2 mTorr CH 3 I from top –15 mTorr Ar from bottom/side –0.060 A (640 V) DC discharge 69 th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. ClZnCH 3 Direct Absorption Spectrum Frequency (MHz) K Components 69 th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. The Search for 66 Zn and 37 Cl Isotopologues 69 th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. Table of Frequencies ClZnCH 3 (v = 0)ClZnCH 3 (v = 1)ClZnCH 3 (v = 2) J′←J″Kν obs ν obs-calc ν obs ν obs-calc ν obs ν obs-calc …… …… … … 230 – 300 GHz 10 transitions of ClZnCH 3 (v = 0,1) 4 transitions of ClZnCH 3 (v = 2) 69 th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. Spectroscopic Constants ClZnCH 3 (v = 0)ClZnCH 3 (v = 1)ClZnCH 3 (v = 2) B (20) (14) (17) DJDJ (32) (23) (36) D JK (12) (10) (14) H JK 0.102(19)x (17) x10 -7 … rms th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. Preliminary ClZnCH 3 Structure 69 th Symp. on Molec. Spectrosc. June 18, Å ClZnCH 3

June 22, th Symp. on Molec. Spectrosc. ClZnCH 3 Formation: Zinc Insertion 69 th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. ClZnCH 3 Current Problem “Searches for the 37 Cl, 66 Zn, 13 C, and D substituted isotopologues are currently in progress.” Expensive –CH 3 Cl (≥99.5%) 1.8 kg for $ –CD 3 Cl (99.5%) 1 L for $ – 13 CH 3 Cl (99%) 1 L for $ mm FTMW 69 th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. Future Work Finish isotopic substitutions for ClZnCH 3 –Cl 66 ZnCH 3 –ClZn 13 CH 3 –ClZnCD 3 – 37 ClZnCH 3 ClMgCH 3 J. Organomet. Chem., 2006, 691, 4341– th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. Thanks to…  Prof. Lucy Ziurys  Ziurys Group  Dr. Gilles Adande  DeWayne Halfen,Jessica Edwards, Jie Min, Julie Anderson, Debbie Schmidt  Funding  NSF  NASA 68 th Symp. on Molec. Spectrosc. June 19, th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. ClZnCH 3 Problem #3: CH 3 Cl 69 th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. The Activation Strain Model 69 th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. ClZnCH 3 Problem #2: Contaminants 69 th Symp. on Molec. Spectrosc. June 18, 2014

June 22, th Symp. on Molec. Spectrosc. 69 th Symp. on Molec. Spectrosc. June 18, 2014