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James Nottage
Birth place or City of origin:
State of origin: WY
Last known City: Indianapolis
Last known State: IN
Death/End date:
James H Nottage, Vice President and Chief Curatorial Officer, has been with the Eiteljorg Museum in Indianapolis, IN since September 2001. Previously he was founding Chief Curator at the Autry Museum of Western Heritage in Los Angeles. He has curated or developed more than 100 special exhibitions. Nottage holds bachelor's and master's degrees from the University of Wyoming and a master's in Museum Studies from the Cooperstown Graduate Program. He is also a graduate of the Getty Leadership Institute for Museum Management. Nottage has edited, authored or contributed essays to a dozen books and publishes frequently in historical journals and magazines.
James is a community associate, Indiana University/Purdue University, Indianapolis (IUPUI). Nottage was founding Chief Curator at what is now the Autry National Center in Los Angeles. He has curated more than 100 special exhibitions and edited, written, or contributed essays to a dozen books, while contributing to many other volumes, including Jewish Life in the American West (2002), How the West Was Worn (2001), and Powerful Images: Portrayals of Native America (1998). James authored "Saddlemaker to the Stars: The Leather and Silver Art of Edward H. Bohlin" (1996), and the recently published, Generation, The Helen Cox Kersting Collection of Southwestern Cultural Arts (2010).
Special thanks to the University of Wyoming for Mr Nottage's 2011 Outstanding Alumnus award, they published the following bio:
James H. Nottage - 2011 Outstanding Alumnus
Bachelor of Arts - 1972 - History
Master of Arts - 1976 - American Studies
A passionate student of the art and people of the American West, James H. Nottage is considered by many an expert in American Indian history and the art and material culture of Western North America. Nottage developed an interest in history and art of the west at a young age, even as early as junior high school. "I was fascinated with real things, objects that could tell me about the past and the people who owned, used, or created them," he explains. "The process of studying and understanding things by examining their design, fabrication, and connections with larger ideas of human creativity and culture has stayed with me ever since."
Nottage, a Laramie native, received a bachelor's degree in History in 1972 and a master's degree in American Studies in 1976 both from UW. Throughout his professional career as a curator and administrator, Nottage has played an important role in helping to expand or create several distinguished cultural institutions, including the Autry National Center, an intercultural history center in Los Angeles; the Kansas Museum of History in Topeka; and the Eiteljorg Museum of American Indians and Western Art in Indianapolis, where he currently serves as vice president, chief curatorial officer, and Gund curator of western art, history, and culture.
Nottage maintains his dedication to the liberal arts and sciences by advancing public museums so that others might learn about diversity in American life through Western history and art. "The humanities provide many opportunities for stimulating careers," he notes. "From them have come professors, judges, curators, authors, teachers, politicians, and others who have enriched all our lives and are far more distinguished than I."
In 1973, Nottage was a graduate research fellow at the Smithsonian Institute where he focused on Plains Indian Art and material culture. He later earned a master's degree in history museum studies from the Cooperstown Graduate Program, the premier programs in the United States that trains museum professionals. Nottage has written, edited, or contributed to more than two dozen books and exhibition catalogs and contributes frequently to magazines and journals of Western history and art. A frequent lecturer, he also has served as an on-camera commentator in numerous documentary films about the American West. "Western history is not just about cowboys and Indians like portrayed in popular media," says Nottage. "There is so much more to understand; it is about diversity of people, of thought, of environment, and of expression."
Nottage acknowledges his intellectual debts to E.B. "Pete" Long and T.A. Larson and also to Herb Dieterich and Robert Righter whose passionate teaching inspired Nottage through his UW master's degree program.


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262-923-8761 24 Hour Emergency Contact
Providing Aggressive, Creative and Comprehensive Criminal Defense
New legislation looks at 'mens rea' in criminal justice: Part I
On behalf of Buting, Williams & Stilling, S.C. posted in Criminal Defense on Thursday, January 21, 2016.
Most of us would consider ourselves law-abiding citizens. But can we be sure? By some estimates, there are approximately 4,500 or more crimes on the books, and that's just at the federal level. And because there is no central database (which would seem like a no-brainer), there is no way to definitively quantify the number of criminal statutes.
With so many potential ways to commit a crime, any of us could be criminals and not know it. This prompts a question that has long been debated in the criminal justice system: Should you be considered guilty by committing a certain act, even if you didn't know the law and had no criminal intent?
Historically, in the United States and elsewhere, crimes generally required two criteria. The first was committing the act itself. The second was a concept called "mens rea," which loosely translates as "guilty mind." In short, an act was considered a crime if it was illegal and if the person committing it knew the law and acted with criminal intent.
Intent is vitally important to discern for certain crimes. If you discharge a gun and kill someone, it obviously matters a great deal whether you did it on purpose or whether it was an accident. The consequence for the victim is the same either way, but your guilt or innocence under the law hinges on mens rea.
But there are many laws on the books that disregard intent or are silent on the issue of intent. For these offenses, ignorance of the law is generally not an acceptable defense. Should that be the case, though? If you are fined for parking in an area with a "no parking" sign, should it matter whether or not you saw the sign?
In late 2015, both houses of Congress introduced bills touted as mens rea reform. If passed, they could significantly change the standards by which federal crimes could be prosecuted in the United States.
Please check back next week as we continue this discussion.
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"The outcome was amazing, one unavailable even under identical circumstances in probably 98 percent of federal courtrooms around the country. Separate and apart from the outcome, though, I am supremely impressed by your efforts on your client's behalf. Your comments in support of the requested sentence were perfect in tone and, having now reviewed the extensive sentencing memorandum you filed, your work in that regard was exemplary as well. Your client was certainly fortunate to have you as his attorney." (Local federal court attorney present at a sentencing)
"I can't thank you enough, not only for all of the tireless work that you and your staff put into my case, but for telling me what I needed to hear, at a time when I absolutely had to hear it. I consider myself blessed for everything turning out the way it did, especially since I blindly picked you out of a phone book! You helped me, my family and friends in many more ways than the money ever could." (Child pornography client)
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If your reading this article you are probably in what we call the 10% of mindset or those in law enforcement that are continually improving themselves both physically and mentally. This article is preaching to the choir, but as members of this proverbial choir your voices need to be heard and you need to sing out loudly to those who are not so concerned about improving themselves as they are jeopardizing your life, the lives in the communities you serve, and the tranquility in a free society that is being torn apart by those that would destroy us. Police officers are the fine blue line between chaos and order. You are our first line of defense.
Today's law enforcement officer can no longer be what has been referred to as a "ROD". That is "Retired on Duty." Those who look at law enforcement as just a paycheck and a career leading to a secure retirement need to be not only shaken, but steered either out of their departments or quickly change their attitude about what it means to be a cop. The risks today are far too great and too treacherous to have anyone that is not at the top of their game. Any athlete of quality who understands that their performance involves mindset, attitude, skills and long term preparation, would not think of the demands of game day long before game day itself. For cops, everyday is game day and being prepared is not just winning, but survival. Last year 162 police officers lost their lives in the line of duty. Already this year 12 officers were shot in one weekend, 53 officers shot at in the month of January alone and the death toll continues to rise. Those who wear the uniform and badge are a symbol of government. Police officers are a virtual target to those who oppose the American way of life be they terrorist, anarchist, gang member, drug cartel or lone wolf.
We have learned through hundreds of conversations with cops that officers talk a lot about "officer safety." The "talk" stems around safety in numbers or staffing, back-up, contact cover principle, cover and concealment, firearms training, situational awareness, recognizing the signs and signals of crime and danger, reading body language, decision making under pressure, active shooter response, hostage negotiation, barricaded subject response, tactical response and approach to calls, off duty survival and many more tactical concepts as well. Talking about the concepts behind officer survival is great, BUT IT'S NOWHERE NEAR ENOUGH! The concepts behind officer survival must be practiced and integrated into every aspect of officer mind set, attitude and personal approach to their duties.
How many of us apply these officer survival concepts on the street? How many of us take short cuts or fall into a complacent mindset and daily routine? How many think 'it will not happen to me' or 'it will not happen here'? We ask you this question: Is officer survival just a concept or have you internalized these safety principles into your habits every day and on every shift? The need for change is obvious, threats are real and evolving despite the fact that most people would never do harm to us. There are still those who, for whatever their personal agenda and reasoning, know we as American guardians are, what we as American Law Enforcement do, and they will unleash their rage and fury at us according to that personal agenda.. The fact that few organized aggressors would resort to mass violence, and many more unplanned, opportunistic or event related aggressors act against Law Enforcement is all the more reason we must develop a mindset of heightened superior situational awareness and mental attitude, while simultaneously being approachable and engaged with those whom we serve and interact. This is true no matter where we are and no matter what we are doing.
Talk is cheap and its time we started walking our own talk and applying the concepts we say are so near and dear to our survival. In the end it comes down to doing the things we talk about; continual learning; and applying what we know to the evolving situation at hand. This takes effort in leadership ensuring proper realistic training is brought to officers, and that LE personnel be open to ongoing professional development, honing of skills, attitude and preparedness through their own individual initiative. If each officer took the responsibility for assuring their survival through ongoing developing, training, and evolution; their entire organization is optimized for survival and adaptive response to threats. It's time to stop merely talking and learn to discipline yourself to walk the walk of officer safety by doing what you know is necessary, and by seeking out more training so you consistently strive to nurture what you know and evolve your skills to be adaptable and instinctive. You do not need to be in formal training class to create and nurture this mindset, indeed it must come from within. It must come from one's own sense of integrity and personal anima and believe system. When this belief system is a way of life, the development occurs as part of an ongoing evolution of a warrior or modern knight.
Several forms of thinking play a crucial role in preparing and readying us for conflict, violence or crisis. These include the "if – then, the when X happens, they Y"… and "what do I do and do I…" effort at anticipating threats as we try to plan for a response to a predator we can't full anticipate..
We need to become students of human behavior, both normal and aberrant, to rapidly recognize the difference between the two and be ready to instantly respond correctly and accurately. Inherent in this is understanding the various dimensions of aberrant behavior between deviant, dangerous, suspicious, under the influence, and psychiatric.
A simple and recognized concept is the Boyd Cycle, which includes Observe-Orient-Decide-Act elements. Commonly referred to as "OODA Loops," this is a concept that applies to everything we do. No matter what we are doing this concept is part of how we learn about what's going on, make decisions as to how to handle it and take actions to effectively and safely get it done. Obviously it takes physical skills as well and time must be spent developing these skills, but by and large, it's lack of awareness or complacency and lack of good sound decision-making that gets us killed in the field. Yes the bad guy has something to do with it, but the fact is we know they are out there stalking the public and cops. The bad guy watches us, learns our habits, and plans his actions and when the opportunity presents itself the bad guy puts his plan into action. His planning and plotting give him an advantage because he is putting an effort forward and walking his own talk. We should be aware of, prepared for and ready to prevent this type of advantage from developing. We need to be thinking in the same way as the bad guy, and do what we call personal "Red Teaming". This means thinking of how we might be compromised and if you yourself were the bad guy how would you aggress or act in a given situation.
Winning takes constant superior situational awareness and a willingness to step outside the lines of traditional training. It requires each of us to use individual insight and innovation in applying what we have learned in training and through our experiences to what we know. Applying what we know then takes consistent and constant practice and "practicing what we preach" to our daily duties. We can no longer be complacent watching cops die, making the same mistakes time and time again. These mistakes are fixable! It's time to call to arms and to wake-up every law enforcement officer to the mindset of survival in the context of where we are now, in a current environment of multiple and chronic threat. It is time to take the mindset that each of us must be one of the 10% who diligently and continually try to improve themselves, optimize our own chances for effective response and survival from threats of all kinds. That warrior mindset, that approach of the knight guarding the kingdom, needs to be the goal of our profession and obligation to serve.
If you knew that tomorrow you were going to be in a gun fight, if tomorrow your community would be hit with a Mumbai type terrorist attack or your child's elementary school was being attacked by terrorists, how would you train today and how would you prepare yourself for tomorrow? Tomorrow may be sooner than we think. Train hard, be aware, stay oriented, and be safe. Evolve to the every-prepared and evolving state-of-the-art modern knight.


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European Maritime Finance (EMF) and the American Club welcome new US Ambassador to Denmark Alan Leventhal.
The event was held in Copenhagen to honor the newly appointed US Ambassador to Denmark Alan Leventhal and his wife Sherry celebrating the American Club's 102nd anniversary, the second oldest American Club in the world.
Ambassador Leventhal was credentialed as the United States Ambassador to the Kingdom of Denmark by Her Majesty Queen Margrethe II on July 1, 2020. Before he was appointed Ambassador, Leventhal was the Chairman and Chief Executive Officer of Beacon Capital Partners. He previously served as President and CEO of Beacon Properties Corporation, a publicly traded real estate investment company.
Leventhal is the former Chair of the Board Damon Runyon Cancer Research Foundation where he also served on the Executive Committee. He was an Executive Committee and life member of MIT and Trustee Emeritus of Boston University where he served as Chair from 2004 to 2008. Leventhal was a life trustee of Northwestern University and also served on the boards of the Friends of Post Office Square and the Norman B. Leventhal Map and Educational Center at the Boston Public Library.
Representing the global shipping investment firm was Martin Haugaard, CEO of European Maritime Finance, Stephen Schueler, President of the American Club Denmark and Chairman of European Maritime Finance, and Torben Bager, Board Advisor to EMF.
Leventhal received his Bachelor's degree in Economics from Northwestern University and a Master's of Business Administration from Dartmouth College. He is married to Mrs. Sherry Leventhal of New Orleans, Louisiana, and together they have six children and 12 grandchildren.
Martin Haugaard, CEO of European Maritime, and Chairman, Stephen Schueler welcomed the new Ambassador to Denmark. Performing during the evening was double Grammy Award winner Mads Tolling, also participating in the Principal Ballerina of the Royal Denmark Ballet and Knighted by the Queen of Denmark, Holly Dorger. Torben Bager, Board Advisor, European Maritime Finance.
Ambassador Leventhal talked about the importance of international trade and have a strong relationship with Denmark. European Maritime's CEO Martin Haugaard said, "Being the sponsor of this prestigious event was in recognition of the fact that European Maritime Finance is committed to global trade, especially between Denmark and the United States. European Maritime is focused on sustainability through the most advanced fuel-efficient vessels." Schueler, also President of the American Club Denmark noted, "we are fortunate to have Alan Leventhal as our U.S. Ambassador building on the strong foundation of the United States and Denmark's collaboration."
About EMF:
European Maritime is a corporate finance company. Focused on direct investments in maritime commercial vessels, ports, and infrastructures. Our current portfolio is well diversified and we continuously seek to expand within traditional shipping segments. We actively support the industry's transition to cleaner fuel improving the environment for future generations and enabling global commerce.
European Maritime Finance Chairman Stephen Schueler participates in the SEB Nordic Investor conference with industry leaders including Gram Car Carriers
European Maritime Finance participated in the SEB annual with global company leaders including Gram Car Carriers. Gram Car Carriers is one of the largest global (...)
European Maritime Finance launches Green Electric Car Carrier (PCTC) investment 3 with a Scandinavia road show.
December 7, 2022·
European Maritime Finance partnering with Atlas Maritime launches the third Green Car Carrier investment project with a Scandinavia Road Show. The first event was held (...)
The event was held in Copenhagen to honor the newly appointed US Ambassador to Denmark Alan Leventhal and his wife Sherry celebrating the American Club's 102nd (...)
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Israel's opposition leader fails to form coalition government
Benny Gantz's lack of success pushes country closer to third round of elections in a year
Oliver Holmes in Jerusalem
Wed 20 Nov 2019 14.39 EST First published on Wed 20 Nov 2019 13.19 EST
The Blue and White party leader, Benny Gantz, had a month to form a coalition. Photograph: Amir Cohen/Reuters
Israel's opposition leader, Benny Gantz, has failed to form a government, increasing the likelihood of the country holding an unprecedented third round of elections.
Gantz had close to a month to forge a coalition after the prime minister, Benjamin Netanyahu, failed to do so. Neither leader won a clear majority during a September election and both have sought to stall each other's play for power.
Under Israeli law, midnight on Wednesday was the deadline, after which Gantz was obliged to return the mandate to the president, Reuven Rivlin. The former Israeli army chief told Rivlin four hours before the deadline that he had not succeeded, his Blue and White party said in a statement.
Politicians loyal to Netanyahu had blocked his attempts, Gantz said in a speech on Wednesday evening, "insisting only on the best interest of one person". Gantz added he had sought to reach out to the prime minister, but his efforts had been met with "insults, slander and childish videos", referring to Netanyahu's frequent social media rants.
Gantz's failure does not automatically trigger elections. It kicks off a final 21-day period in which the Knesset, Israel's parliament, can nominate any candidate to be prime minister, including Netanyahu or Gantz. However, the divided makeup of the Knesset would lead to a tough battle as no political alliance has a majority of 61 seats. After that period, Israelis will be on course to go to the polls again, the third time in a year.
In May, Netanyahu failed to cobble together a coalition following April's muddied election result. A second election was held in September, but the ballot only delivered a similar result.
The political stalemate has played out during a fraught time for Israel as an increasingly open conflict heats up with Iran, its arch-enemy and a regional powerhouse.
Israel's military said on Wednesday its jets had bombed dozens of Syrian and Iranian targets overnight in neighbouring Syria. The British-based monitoring group the Syrian Observatory for Human Rights said 23 people had been killed in the strikes, 21 fighters and two civilians.
Rivlin had been pressing the two main parties to put aside their differences and form a unity government as they would have more than enough seats for a majority. But there have been vast differences between the rivals during negotiations on key aspects such as how the next administration will look, including who leads it.
Gantz ran his election campaign on the promise to topple Netanyahu, making it difficult for the opposition leader to accept a power-sharing deal without losing credibility.
Meanwhile, the prime minister has insisted his traditional allies from hardline nationalists to religious parties be included in any unity government, a precondition Gantz has rejected.
Netanyahu also faces the possibility of court cases that could lead to jail time. Israel's attorney general is deciding whether to indict him in three potential corruption cases. If he retains the role of prime minister, he will not be required to step down, even if indicted, and could use his position to push for immunity. Netanyahu has denied all allegations.
Gantz had several ways of forging a coalition, including the possibility of courting politicians from Israel's Arab minority, which makes up close to a fifth of the country's population.
To block this route, Netanyahu has claimed that a government propped up by Arab parties would be a "historic danger to Israel's security" and accused Arab politicians of allegiance to Palestinian militant groups.
Rivlin, who is tasked with overseeing the government formation, strongly rebuked Netanyahu for the campaign. "The characterisation of all Arab elected officials as a 'threat' to the existence of the state of Israel and as a 'fifth column' must be emphatically denounced," he said this week.
Israel heading for unprecedented third election in a year
New election will be held in March unless rivals can break political deadlock by midnight
Netanyahu rivals move to bring him down after corruption indictments
Israeli opposition parties scramble to find legal channels to strip weakened PM of power
Israeli PM Benjamin Netanyahu indicted for bribery and fraud
Attorney general announces charges as crisis deepens for longest-serving leader
Israeli president tells parliament to find new PM or face election
Benjamin Netanyahu and rival Benny Gantz have each failed to form a government
Israel opposition leader nears deadline to form coalition government
Benny Gantz tasked with forming Israeli government
Benjamin Netanyahu tells Israeli president he cannot form government
Crunch time for Netanyahu as talks with rival politicians break down
More more on this story


Korby Lenker is a sneaky-good songwriter. And singer. And multi-instrumentalist. An abbreviated list of Lenker's achievements so far includes: a significant amount of airplay on the legendary Seattle indie rock station KEXP; a BBC 2 interview with Bob Harris, which is only about the highest honor a rootsy singer-songwriter touring the U.K. can get; opening slots for acts ranging from Willie Nelson to Ray LaMontagne, Nickel Creek, Keith Urban, Susan Tedeschi and Tristan Prettyman; a successful run with one of the hottest young West Coast bluegrass bands of the aughts; and wins in the Merlefest folk songwriting contest as well as the Kerrville Folk Festival's elite New Folk songwriting competition.


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Q: Can I transfer secondary OS to ssd drive? I am running dual boot centos/windows.
Is it possible with lVm to migrate the linux partitions from hdd to ssd?
If possible a summary of what needs to be done or links to guides for 'how to'?
(Not a windows question)

A: Thanks for the tips from the peanut gallary.  I did google the revised question and found How do I move my LVM  ...

redpajama_set_name: RedPajamaStackExchange


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Micheaux, Oscar
Race films
Spence, Louise
Writing Himself Into History: Oscar Micheaux, His Silent Films, and His Audiences
by Pearl Bowser and Louise Spence
Rutgers University Press, 2000
eISBN: 978-0-8135-6044-1 | Cloth: 978-0-8135-2802-1 | Paper: 978-0-8135-2803-8
Library of Congress Classification PN1998.3.M494B69 2000
Dewey Decimal Classification 791.430233092
Winner of the 2001 Kraszna-Krausz Moving Image Book Awards | Winner of the Theatre Library Association Award
Writing Himself Into History is an eagerly anticipated analysis of the career and artistry surrounding the legendary Black filmmaker Oscar Micheaux. With the exception of Spike Lee, Micheaux is the most famous—and prolific—African American film director. Between 1918 and 1948 he made more than 40 "race pictures," movies made for and about African Americans. A man of immense creativity, he also wrote seven novels.
Pearl Bowser and Louise Spence concentrate here on the first decade of Micheaux's career, when Micheaux produced and directed more than twenty silent features and built a reputation as a controversial and maverick entrepreneur. Placing his work firmly within his social and cultural milieu, they also examine Micheaeux's family and life. The authors provide a close textual analysis of his surviving films (including The Symbol of the Unconquered, Within Our Gates, and Body and Soul), and highlight the rivalry between studios, dilemmas of assimilation versus separatism, gender issues, and class. In Search of Oscar Micheaux also analyzes Micheaux's career as a novelist in relation to his work as a filmmaker.
This is a much-awaited book that is especially timely as interest in Micheaux's work increases.
Pearl Bowser, founder of the African Diaspora Images collection, specializes in African and African American film. She co-directed the award-winning documentaryMidnight Ramble: Oscar Micheaux and the Story of Race Movies. Louise Spence is an associate professor and coordinator of media studies at Sacred Heart University in Connecticut and has published extensively in scholarly journals and anthologies.Thulani Davis is a writer, author of the novels Maker of Saints and 1959 and contributor to Malcolm X: The Great Photographs and the biographical film W.E.B. Du Bois.
See other books on: 1884-1951 | Audiences | Micheaux, Oscar | Race films | Spence, Louise
See other titles from Rutgers University Press
Nearby on shelf for Literature (General) / Drama / Motion pictures:


You will be assigned to our Widnes Jewson branch and required to cover a cluster of branches.
These branches are; Widnes, Wigan, St Helens,Warrington, Wallasey and Birkenhead.
You will receive mileage payments for when travelling to these other branches.
On top of your basic salary you'll receive a subsistence and mileage.


Birth Doula in the Permian Basin area. This area includes Midland, Odessa, Crane, Kermit, Pecos, Fort Stockton, Monahans, Andrews, and other surrounding cities (all in Texas).
If you are needing a doula from another part of the country, please venture over to my Links page. There, you will also find links to local resources and other doulas in our area. If, while visiting the pages of other doulas, you see a service offered that you want, please let me know. I will do everything I can to help you have your desired pregnancy and birth!


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New Website Launched
Mocha Violet is proud to announce the launch of our new website! Your inspiration awaits…
New Website Launched : Read more
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Mocha Violet
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The Olney Help Food Drive is a community project sponsored by the third grade to help needy families in our area. It is being held from 11/4 thru 11/22. Acceptable items of donations are any non-perishable foods-boxes, bags, cans, or jars. Students should bring their donations to their classroom. Our school goal is to collect 600 items!
The food will be used to feed hungry families in the greater Olney area. Olney Help says their most wanted items are canned foods, such as fruit, tuna, pasta, sauce, vegetables, and baked beans. They also need boxed foods, such as cereal, rice, macaroni and cheese, and potatoes. Thanks in advance for all your donations!


An unorthodox look at the colorful, Byzantine political culture of Louisiana, home to governors like the legendary Huey Long and his brother Earl (who was committed to an asylum during his last term), Jimmie Davis (who sang his farewell to the Legislature), the roguish four-time elected Edwin Edwards and reactionary, racist figures like Judge Leander Perez and David Duke. Earl Long said it best in the 1950s: "One of these days Louisianans are going to get good government...and they ain't going to like it!" Louisiana Boys: Raised on Politics looks at the history and the condition of this political circus, from the populist tradition of the Longs, the emerging power of Blacks in New Orleans, and the traditional three-way split (conservative-Protestant Northern Louisiana, Cajun-Catholic Southern Louisiana, and urban New Orleans) that has kept the state's political culture a popular spectator sport.
"Louisiana Boys - Raised on Politics" was supported by grants from Louisiana Endowment for the Humanities, the Louisiana Division of the Arts, the Southern Educational Communications Association, and the Mary Freeman Wisdom Foundation.
A production of The Center for New American Media and Midnight Films. Winner of the Silver Baton, Alfred I DuPont-Columbia University Award.


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Journal of Inorganic and Organometallic Polymers and Materials
January 2020 , Volume 30, Issue 1, pp 196–205 | Cite as
Synthesis of Unsymmetrical Bis(phosphine) Oxides and Their Phosphines via Secondary Phosphine Oxide Precursors
James R. Pedroarena
Bryan P. Nell
Lev N. Zakharov
David R. Tyler
First Online: 21 August 2019
The unsymmetrical bidentate phosphine ligands (Me)2PCH2CH2CH2P(Et)2 (14), (Me)2PCH2CH2CH2P(iPr)2 (15), (Me)2PCH2CH2CH2P(Cy)2 (16), and (Me)2PCH2CH2CH2P(Ph)2 (17) were synthesized using air–stable phosphine oxide intermediates. In the first step, sodium phosphinites formed by deprotonation of (Me)2P(O)H, (Et)2P(O)H, and (iPr)2P(O)H were alkylated by 1-bromo-3-chloropropane. The different substitution rates of the chloride and bromide groups allowed the isolation of the intermediates (Me)2P(O)CH2CH2CH2Cl (2), (Et)2P(O)CH2CH2CH2Cl (3), and (iPr)2P(O)CH2CH2CH2Cl (4). Subsequent reaction of (Me)2P(O)CH2CH2CH2Cl (2) with the sodium phosphinites generated from (Et)2P(O)H, (iPr)2P(O)H, (tBu)2P(O)H, (Cy)2P(O)H, or (Ph)2P(O)H gave unsymmetrical bidentate phosphine oxides; reduction of these oxides yielded the unsymmetrical phosphines. The unsymmetrical bidentate phosphines react with metal salts to form complexes. X-ray crystal structures of cis-Pt((Me)2P(CH2CH2CH2)P(iPr)2)Cl2 (20) and racemic [CuI((Me)2P(CH2CH2CH2)P(Ph)2)]Cl (21) were obtained. The kinetics and scope of the synthetic route were also explored. Experiments showed that the rate of substitution of the alkyl chloride group in (R)2P(O)CH2CH2CH2Cl-type oxides increases relative to unsubstituted alkyl chlorides due to the presence of the phosphonyl group on one end of the molecule. The scope of the reaction involving 1,2-dihaloalkanes was also investigated, and it was found that the reaction mixture of sodium dimethylphosphinite and 1,2-dihaloalkanes formed tetramethylbis(phosphine) monoxide (22), which decomposes on work-up to give complex reaction mixtures.
Unsymmetrical phosphines Unsymmetrical phosphine oxides Phosphine ligands Phosphinite anions Heteroleptic phosphines
Bidentate ligands have found extensive use in transition metal catalysis, including use in the preparation of polymer materials [1, 2, 3, 4].
Bidentate ligands can either be symmetric or unsymmetric. For example, the bidentate ligands in Fig. 1 are symmetric (DPPE [5] and DPPF [6]) or "C2-symmetric" (DIOP [7], BINAP [8], and DUPHOS [9]). The donor atoms on symmetric and C2-symmetric bidentate phosphine ligands all possess the same carbon groups, which means that the electronic and steric properties at each phosphorus center are the same [10]. In contrast, bidentate ligands can have different groups bonded to the donor atoms, making them unsymmetrical. Many examples of unsymmetrical ligands exist, notably: salen ligands (N donor atoms) [11], bypyridine and other bidentate pyridine ligands [12, 13], phosphine–carboxylate ligands [3], phosphine–carboxylate ligands [1], phosphine–phosphine oxide ligands [14], phosphine–phosphite ligands [15], phosphine–phosphinite ligands [15], and NHC ligands [16]. However, it is uncommon to encounter unsymmetrical phosphine–phosphine ligands [17, 18, 19, 20, 21, 22, 23, 24, 25]. Unsymmetrical phosphines are rare due to their lengthy syntheses as a result of the necessary stepwise addition of the −PR2 groups to the backbone and the use of pyrophoric secondary phosphines and chlorophosphines [17, 18, 19, 20, 21, 22, 23, 24, 25]. Such ligands may have use in tuning catalysts by providing two electronically and sterically different donor phosphorus atoms [25]. Unsymmetrical ligands can potentially convey intermediate properties to metal centers compared to symmetric ligands, and thus easier syntheses of them would allow for exploration of their ability to tune catalysts.
Examples of symmetric and C2-symmetric phosphine ligands
There are several applications of unsymmetrical ligands. For example, nickel and palladium catalysts with phosphine–imine ligands for ethylene polymerization have been shown to perform as well as and have higher temperature stability than analogous catalysts with imine–imine ligands [3]. Furthermore, the activity of the palladium-catalyzed asymmetric copolymerization of propene and carbon monoxide benefits from the use of an unsymmetrical chiral phosphine–phosphite ligand [2]. Additionally, the use of unsymmetrical phosphine–phosphite [26], phosphine–phosphinite [26], phosphine–imine [27], phosphinite–imine [27], and phosphine–phosphine [25] bidentate ligands in asymmetric catalytic processes can increase stereoselectivity. Finally, it is also noted that bidentate phosphine ligands are capable of forming coordination polymers with interesting properties [28, 29, 30]. Unsymmetrical bidentate phosphines are potentially useful in tweaking the properties of these materials.
The development of synthetic routes to tertiary phosphines via air–stable intermediates and easier workups has been of great interest to our research group [31, 32]. In this work, we demonstrate the synthesis of unsymmetric bidentate phosphines utilizing air–stable phosphine oxide starting materials and intermediates. The synthetic route [32] employs nucleophilic phosphinite anions, generated by deprotonation of secondary phosphine oxides (SPOs) with sodium hexamethyldisilazide (NaHMDS), followed by the alkylation of the anions with alkyl halides to form tertiary phosphine oxides, Scheme 1 [32].
Deprotonation and subsequent alkylation of SPOs using NaHMDS
In prior work [32], we showed that the phosphinite anions displayed reactivity suggestive of an SN2-like mechanism, as indicated by their sensitivity to steric constraints and by their reactivity with alkyl halides following the trend RI > RBr > RCl. The observed regioselectivity allowed for isolation of (Me)2P(O)(CH2)3–5Cl species and subsequent reaction to form unsymmetrical bis(phosphine) oxides (Me)2P(O)(CH2)3–5P(O)(t-Bu)2 [32], Scheme 2.
Synthesis of unsymmetrical bis(phosphine) oxides [32], n = 1–3
In this study, we extend our prior work to include the synthesis of (R)2P(O)CH2CH2CH2Cl, (Me)2P(O)CH2CH2CH2P(O)(R)2/(Et)2P(O)CH2CH2CH2P(O)(iPr)2 (where R = Et, iPr, t-Bu, Cy, Ph), (Me)2PCH2CH2CH2P(R)2, and several metal complexes with the unsymmetrical phosphine ligands. To our knowledge, this is the first report of unsymmetrical bidentate phosphine ligands synthesized using only air–stable starting materials and intermediates. In order to demonstrate the coordination chemistry of these ligands, two X-ray crystal structures of the metal complexes with unsymmetrical ligands were obtained. Additionally, the kinetics and the scope of the synthetic route were investigated.
2.1 (3-Chloropropyl)dialkylphosphine Oxides, (R)2P(O)CH2CH2CH2Cl
Synthesis of the (3-chloropropyl)dialkylphosphine oxide (precursors to the unsymmetrical bis(phosphine) oxides) was carried out following the reaction conditions shown in Scheme 3.
Reaction of the phosphinite anion with 1-bromo-3-chloropropane
Very low yields of the mixed alkyl halide phosphine oxides products were obtained in our early study of the reactions of phosphinite anions with 1-bromo-3-chloropropane. The low yields for the reactions were attributed to loss of the product in the aqueous phase during the extraction process due to the water-solubility of the product. However, isolation of the disubstituted product (Me)2P(O)CH2CH2CH2P(O)(Me)2 (1; 62% yield; Scheme 4) demonstrated that the low yields were the result of subsequent substitution at the alkyl chloride position after the initial substitution of the bromide. (Similar disubstituted products were also found in every other reaction of a phosphinite anion with 1-bromo-3-choropropane.) Substitution of the chloride is contrary to the observations in our previous study [32], which suggested little to no substitution would occur at the chloride position in the time it would take to substitute the bromide. The comparable rates of reaction observed in the current study may be due to the presence of the phosphonyl group near the alkyl chloride, which could stabilize the transition state by interacting with the Na+ counterion (Fig. 2a). Alternatively, the sodium counterion may associate closely with the oxygen atom of the phosphonyl group, leading to a preferred encounter between the phosphorus atom and the alkyl chloride (Fig. 2b).
Formation of the symmetrically substituted bidentate product leads to lower yields of the alkyl chloride phosphine oxides
Hypothesized reasons for the increased rate of the substitution reaction of (3-chloropropyl)dialkylphosphine oxides. a In this hypothesis, interaction of the oxygen atom of the phosphonyl group with the Na+ ion stabilizes the transition state. b In this hypothesis, complexation of the sodium cation by phosphonyl increases the likelihood of the substitution reaction
In order to overcome the low yields, a slight excess of 1-bromo-3-chloro propane was used and the phosphinite anions were added slowly to the solution of 1-bromo-3-chloropropane. (Note that addition of the phosphinite anion to the reaction solution is opposite to the procedure in our previous work [32]. Addition of the phosphinite to the 1-bromo-3-chloro propane led to respectable increases in the yields, Table 1.)
(3-Chloropropyl)dialkylphosphine oxides
Yield (%)a
aAverage of two isolated yields
In addition to the three oxides in Table 1, attempts were made to generate and isolate the di-tert-butyl-(5) and dicyclohexyl-(6) substituted (3-chloropropyl)dialkylphosphine oxides (Fig. 3). However, these molecules could not be reliably separated at a sufficient purity from the impurities in the reaction mixtures.
Product molecules 5 and 6 that could not be purified reliably. These molecules would require larger scale reactions in order to separate the impurities which are very similar in polarity, solubility, and boiling point
It is of note that in almost every case, crude material obtained from the reaction of one of the phosphinite anions with 1-bromo-3-chloropropane contained a small amount of (3-bromopropyl)dialkylphosphine oxide product (7; Fig. 4). However, formation of 7 was not an issue because only a minor amount formed, and it was easily separated by distillation. A crystal structure of the (3-chloropropyl)dimethylphosphine oxide species (2) is shown in Fig. 5.
(3-Bromopropyl)dialkylphosphine oxide product (7), a minor product formed during the reaction of sodium phosphinites with 1-bromo-3-chloropropane
ORTEP drawing of 2 with thermal ellipsoids drawn at the 50% level. The H-atoms are omitted for clarity
2.2 Unsymmetrical Bis(phosphine) Oxides
Unsymmetrical bis(phosphine) oxides were synthesized according to the route in Scheme 5.
Reaction of (3-chloropropyl)dialkylphosphine oxides with phosphinite anions to form unsymmetrical bis(phosphine) oxides
Substitution of the chloride in (3-chloropropyl)dialkylphosphine oxides proceeded rapidly after addition to the phosphinite anion solutions. In most cases, the reactions were completed in under 30 min as indicated by 31P NMR spectroscopy. The yields of the bis(phosphine) oxide products are shown in Table 2. Note that the unsymmetrical bis(phosphine) oxides were synthesized in reasonable yields. The (3-chloropropyl)dimethylphosphine oxide starting material was used for all but one of the unsymmetrical oxides, but it should be apparent that any combination of R groups is likely possible on either end of the linker.
Unsymmetrical bis(phosphine) oxides
It is noted that as the solubility of the unsymmetrical bis(phosphine) oxides increases in organic solvents (i.e., as the polarity of the molecule decreases because the R groups get larger) the separation of the unsymmetrical molecules from impurities in the reaction solution becomes more difficult. (For example, compare the work-up for product 13 to those for products 8–12; see Sect. 2) Crystal structures of oxides 8 and 12 were obtained and are shown in Fig. 6.
ORTEP drawings of molecules 8 and 12 with thermal ellipsoids drawn at the 50% level. The H-atoms were omitted for clarity
ORTEP drawings of cis-Pt((Me)2P(CH2CH2CH2)P(iPr)2)Cl2 (20, left) and the cationic portion of [CuI((Me)2P(CH2CH2CH2)P(Ph)2)]Cl (21, right) with thermal ellipsoids drawn at the 50% level. The H-atoms have been omitted for clarity
2.3 Unsymmetric Bidentate Phosphines
The unsymmetrical bis(phosphine) oxides were reduced to their corresponding unsymmetrical bidentate phosphines in mostly good yields following a reduction methodology [33] recently reported by our group, Scheme 6. The phosphines and their yields are summarized in Table 3.
Reduction of unsymmetrical bis(phosphine) oxides
Unsymmetrical bidentate phosphines
bOnly reduction of the PMe2 unit occurred
2.4 Complexes with Unsymmetrical Bidentate Ligands
Several metal complexes were synthesized using the unsymmetrical bidentate ligands, Scheme 7.
Syntheses of cis-Pt((Me)2P(CH2CH2CH2)P(iPr)2) (top; 20) (the cis-Pt((Me)2P(CH2CH2CH2)P(Et)2) derivative (19) was synthesized in the same manner) and [CuI((Me)2P(CH2CH2CH2)P(Ph)2)]Cl (below; 21). The crystal structures of these molecules are shown in Fig. 7
It is interesting to note that the unsymmetrical phosphine ligands cause the copper atom to be an asymmetric center in the [CuI((Me)2P(CH2CH2CH2)P(Ph)2)]Cl complex (21). The crystal structure is centro-symmetric, which means the compound crystallized as a racemic mixture of two enantiomers.
Additional interesting results derived from the X-ray diffraction data are the bond angles and bond lengths of each complex. Diagrams of the bond angles are shown in Fig. 8, and Table 4 shows the M–P bond lengths.
Diagrams of the bond angles in cis-Pt((Me)2P(CH2CH2CH2)P(iPr)2)Cl2 (left; 20) and [CuI((Me)2P(CH2CH2CH2)P(Ph)2)]Cl (right; 21)
M–P and M–X bond lengths for the complexes with unsymmetrical ligands
Cis-Pt((Me)2P(CH2CH2CH2)P(iPr)2)Cl2 (20)
2.243 (2) P1
2.361 (2) Cl1
[CuI((Me)2P(CH2CH2CH2)P(Ph)2)]Cl (21)
2.2740 (9) P1
As one would expect, the unsymmetrical (Me)2P(CH2CH2CH2)P(iPr)2 ligand (15) causes the bond angles in Fig. 8 and the bond lengths in Table 4 for cis-Pt((Me)2P(CH2CH2CH2)P(iPr)2)Cl2 (20) to be different. Likewise, in the case of the tetrahedral copper center in [CuI((Me)2P(CH2CH2CH2)P(Ph)2)]Cl (21), all of the bond angles and bond lengths are different. However, it is odd that the bond angles and lengths are significantly different in the [CuI((Me)2P(CH2CH2CH2)P(Ph)2)]Cl complex (21) even though the two ligands are the same. These differences are due to the chirality of the complex, which requires that the four phosphorus atoms be structurally different. The lack of symmetry in the structures of the complexes demonstrates how different groups on the donor atoms at either end of a ligand can cause significant changes in the coordination environment of metal complexes.
2.5 Brief Investigation of Reaction Scope
It was previously shown that the reaction of sodium dimethylphosphinite and 1,2-dihaloalkanes resulted in complex mixtures of phosphorus products instead of clean conversion to the disubstituted or monosubstituted products (Scheme 8).
Instead of the formation of the expected products, complex mixtures were found upon work-up
This result prevented the synthesis of symmetric and unsymmetric bis(phosphine) oxides with ethene linkers using sodium phosphinites. In this work, synthesis of oxides with ethene linkers was attempted again with 1,2-dihaloalkanes. It was confirmed that the expected products were not formed in a significant quantity, but 31P NMR spectra of the reaction mixtures showed the presence of tetramethylbis(phosphine) monoxide (22) as a major product, based on literature 31P NMR chemical shifts and coupling constants [34]. The 31P NMR spectrum of the crude material from the reaction of 1,2-dibromoethane and 2 equivalents of NaOP(Me)2 is shown in Fig. 9.
NMR of the crude material from the reaction of 1,2-dibromoethane with 2 equivalents of sodium dimethyl phosphinite. The reaction was quenched with 2-butanol and the solvent was removed under vacuum. The dry mixture was suspended in chloroform, filtered, and the solvent removed once again under vacuum
This result explains why the reactions of NaOP(Me)2 with 1,2-dihaloalkanes form complex mixtures upon work-up, namely because the tetramethylbis(phosphine) monoxide decomposes to yield oxidation products upon work-up in air.
Six different unsymmetrical bis(phosphine) oxides (8–13) were synthesized by the route in Scheme 4. There are few previous reports of unsymmetrical bidentate phosphines, and their syntheses involve the use of malodorous and pyrophoric phosphine precursors. The key insight in the route to unsymmetrical phosphines reported here is the use of 1-bromo-3-chloropropane. The different rates of bromide and chloride substitution in this molecule allowed for the isolation of the (3-chloropropyl)dialkylphosphine oxide intermediates. Three examples of (3-chloropropyl)dialkylphosphine oxides (2–4) were synthesized by reaction of sodium dialkylphosphinites with 1-bromo-3-chloropropane. Subsequent reaction of (3-chloropropyl)dimethylphosphine oxide (2) or (3-chloropropyl)diisopropylphosphine oxide (4) with various sodium phosphinites yielded six different unsymmetrical bis(phosphine) oxides (Table 2). Reduction of four of the bis(phosphine) oxides bearing methyl groups on one of the phosphorus centers yielded the unsymmetrical bidentate phosphines, (Me)2P(CH2CH2CH2)P(R)2 (14–17) (Table 3). Two platinum dichloride bis(phosphine) complexes were also synthesized: cis-Pt((Me)2P(CH2CH2CH2)P(Et)2)Cl2 (19) and cis-Pt((Me)2P(CH2CH2CH2)P(iPr)2)Cl2 (20); the X-ray crystal structure of cis-Pt((Me)2P(CH2CH2CH2)P(iPr)2)Cl2 (20) was obtained. In addition, a racemic tetrahedral copper I complex was isolated, [CuI((Me)2P(CH2CH2CH2)P(Ph)2)]Cl (21), and its X-ray crystal structure obtained. A review of the literature reveals that uses for unsymmetrical bidentate phosphines are currently unexplored. But, the method or ligands described here may find use in tuning the electronics and sterics of transition metal catalysts by providing an alternative to symmetrical ligands. The synthetic method reported here is the first report of unsymmetrical bidentate phosphines being synthesized where the final step of the synthesis (the formation of the phosphine) is the only step forming an air-sensitive product. In attempts to make symmetrical and unsymmetrical 1,2-bis(phosphine) oxides via reactions of sodium phosphinites, it was observed that sodium dimethylphosphinite reacted with 1,2-dibromoethane and 1-bromo-2-chloroethane to form tetramethyldiphosphine monoxide (22) among other products. This result implies that an unexpected reaction pathway is occurring other than just nucleophilic attack by the phosphorus or oxygen of the phosphinite.
4 Experimental
4.1 General Procedures and Instrumentation
Unless otherwise stated, all reactions were done under an inert atmosphere of nitrogen in oven-dried glassware. Standard Schlenk techniques were used for all reactions performed outside of a glovebox. Tetrahydrofuran (THF), diethyl ether, hexanes, and acetonitrile were dried using a DriSolv system employing CuO and molecular sieves. The THF, ether, hexanes, and acetonitrile were stored in a glovebox over activated molecular sieves prior to use. Anhydrous glyme was obtained from Acros Organics and stored over sieves in a glovebox. Additional solvents were dried by refluxing over sodium metal overnight, distilling, and then storing over sieves in a glovebox. Pentane was distilled immediately prior to its use in the extractions of the unsymmetrical bidentate phosphines in order to degas it. Diethyl phosphite was obtained from Sigma-Aldrich and distilled before use. 1-Bromo-3-chloropropane was obtained from the Eastman Chemical Company and distilled prior to use or used as received. Lithium aluminum hydride (LAH) was obtained as a pure white powder by removal of solvent from 1.0 M solutions obtained from Sigma-Aldrich or by washing solid gray LAH obtained from Sigma-Aldrich with diethyl ether, filtering the suspension, and removing the diethyl ether under vacuum. All other commercially obtained reagents and solvents were used without further purification unless specified. All synthesized organomagnesium reagents were titrated with salicylaldehyde phenylhydrazone according to the literature [35] and used immediately or stored overnight under N2. Salicylaldehyde phenylhydrazone was prepared according to the literature [35]. Solutions of 2 M sodium bis(trimethylsilyl)amide (NaHMDS) in THF were obtained from Acros Organics and titrated with 9-methyl-9H-fluorene in a modified literature method (see page 13) [36]. Thin-layer chromatography (TLC) was performed on either basic alumina plates for bis(phosphine) oxides or silica TLC plates for mono(phosphine) oxides and SPOs. The basic alumina plates were obtained from Macherey–Nagel. Silica gel 60 F254 plates were obtained from EM Scientific. TLC was visualized with ultraviolet light for aryl species or phosphomolybdic acid stains for alkyl phosphine oxides, which typically resolved as white spots upon heating. 1H NMR spectra were collected on either a 500 MHz Varian spectrometer or a 600 MHz Bruker spectrometer and reported relative to deuterated solvent signals. 1H NMR data is reported as follows: chemical shift (δ ppm), multiplicity, coupling constant (Hz), and relative integration. 13C NMR spectra were collected on a 600 MHz Bruker spectrometer (151 MHz) and reported relative to tetramethyl silane. 31P NMR data were collected on either a 500 MHz Varian spectrometer or a 600 MHz Bruker spectrometer (202 MHz or 243 MHz, respectively) and reported relative to 85% H3PO4. High resolution mass spectrometry (HRMS) data were performed and analyzed by Dr. Felix Grun of the Mass Spectrometry Facility at the University of California Irvine (2, 4, 8–18, 21) and Jeff Morré of the Mass Spectrometry Facility at Oregon State University (19, 20). All samples were within acceptable error. Elemental analyses were done by Complete Analysis Laboratory in Highland Park, New Jersey (3, 11, 13–21) and Atlantic Microlab in Norcross, Georgia (4, 8, 9, and 12).
4.2 General Synthesis of (3-Chloropropyl)dialkylphosphine Oxides (2–4)
A Schlenk flask was charged with an SPO (1 equivalent, ca. 1.3 M) and THF. To the phosphine oxide solution, a solution of NaHMDS (1 eq) was added dropwise at room temperature with stirring. After at least 15 min, the phosphinite anion suspension or solution was added slowly to a ca. 1.3 M solution of 1-bromo-3-chloropropane in THF (1.25 eq) in a Schlenk flask at room temperature. After 2–6 h of stirring at room temperature the reaction was quenched with one volume equivalent of deionized water (equivalent volume to THF used to dissolve SPO) and extracted with one volume equivalent of dichloromethane (DCM) 5–10 times. (Check the explicit syntheses in the Electronic Supplementary Material for the specific number of extractions needed.) The combined organic extracts were dried over sodium sulfate and then filtered. The sodium sulfate was washed with dichloromethane and added to the filtrate. The solvent was removed in vacuo to yield a yellow oil. Purification of the crude (3-chloropropyl)dialkylphosphine oxides was accomplished by either sublimation or a mixture of chromatography and distillation (see explicit syntheses).
4.3 General Synthesis of Unsymmetrical Tertiary Bis(phosphine) Oxides (8–13)
A Schlenk flask was charged with a SPO (1 eq, ca. 0.2 M) and THF. To the phosphine oxide solution, a solution of NaHMDS (1 eq) was added dropwise at room temperature with stirring. After at least 15 min, a solution of a mixed alkyl chloride tertiary phosphine oxide (1 or 3) (ca. 0.2 M) in THF was added dropwise to the phosphinite anion solution/suspension maintained at room temperature. After 2–3.5 h, the reaction was quenched with one or two volume equivalents of deionized water (depending on whether the aqueous or organic phase was collected) and extracted with either ethyl acetate or DCM (depending on which phase was collected, check explicit syntheses). Whichever phase was collected had its solvent removed in vacuo; organic extracts were dried before their solvent was removed in vacuo. The crude material thus obtained was dissolved in 5% methanol/DCM and run through a short plug of basic alumina, which was washed with 50 mL of the methanol/DCM solution. After removal of solvent, the solids thus obtained were washed with cold ether, followed by dissolution and filtration through diatomaceous earth. Removal of solvent yielded a colorless solid (see explicit syntheses for more details; for 9 the workup and purification differs greatly from this general method).
4.4 General Synthesis of Unsymmetrical Bidentate Phosphines (14–18)
A ca. 1.0 M solution of alane (6.4 equivalents) in glyme was prepared from aluminum trichloride (0.2370 g, 1.78 mmol) and purified lithium aluminum hydride (0.2026 g, 5.35 mmol; see the Electronic Supplementary Material for details). A Kjeldahl flask was charged with an unsymmetrical bis(phosphine) oxide (1 equivalent, 0.5 M) and glyme (most of the oxides were insoluble in glyme). A Kjeldahl flask was equipped with an addition funnel and charged with the ca. 1.0 M alane solution. The suspension of the oxide was maintained at room temperature and stirred while alane was added to the mixture dropwise. (The alane solubilizes the oxide and H2 begins forming.) The addition funnel was replaced with a reflux condenser and the reaction heated to 62–68 °C, whereupon a white precipitate formed. After 12 h, gray solids had precipitated, and the reaction was cooled to room temperature and quenched by slow addition of a degassed solution of sodium phosphate (10 equivalents, 0.5 M) in deionized water. (The first few drops were added slowly while the mixture reacted violently with the water.) After 2 h of stirring at room temperature, the mixture was extracted five times by syringe with 10 mL of freshly distilled pentane. The extracts were dried, cannula transferred to a new flask, and the solvent was removed in vacuo to yield a greasy oil. The oil was dissolved in a small amount of hexane and run through a short column of silica and eluted with diethyl ether. After removal of solvent, the oil was dissolved in diethyl ether and filtered through diatomaceous earth. Removal of the solvent yielded the pure phosphine oil.
4.5 X-ray Structures
Diffraction intensities for 2, 8, 12, 20, and 21 were collected at 173 K on a Bruker Apex2 CCD diffractometer using CuKα radiation, λ = 1.54178 Å. Space groups were determined based on systematic absences (2, 12, 20) and intensity statistics (8, 21). Absorption corrections were applied by SADABS [37]. Structures were solved by direct methods and Fourier techniques and refined on F2 using full matrix least-squares procedures. All non-H atoms were refined with anisotropic thermal parameters. H atoms in 8 and 12 were found from the residual density maps and refined without restrictions with isotropic thermal parameters. H atoms in 2, 20 and 21 were refined in calculated positions in a rigid group model. The –CH2–CH2–CH2– group in 2 and one of two solvent CHCl3 molecules in 21 are disordered over two positions in the ratio 1:1. The Flack parameter for 20 is 0.035 (11). All calculations were performed by the Bruker SHELXL-2014 package [38].
Acknowledgment is made to the NSF (CHE-1503550) for the support of this research. The project described was supported, in part, by the Oregon State University Research Office. The content is solely the responsibility of the authors and does not necessarily represent the official views of the OSU Mass Spectrometry Center. The authors acknowledge the OSU Mass Spectrometry Center at Oregon State University and specific institutional instrument grants. Orbitrap Fusion Lumos—NIH #1S10OD020111-01, Waters Ion Mobility ToF Mass Spectrometer—NIH #1S10RR025628-01, Applied Biosystems 4000Qtrap—NIH #1S10RR022589-01, ABSciex Triple ToF 5600—NIH #1S10RR027878-01. Dillon Bryant, Daniel Berg, and Alexi Overland are acknowledged for their contributions to this project.
10904_2019_1288_MOESM1_ESM.pdf (9.3 mb)
The crystallographic data for complexes 2, 8, 12, 20, and 21 are deposited with the Cambridge Crystallographic Data Centre (CCDC 1936444, CCDC 1936443, CCDC 1936447, CCDC 1936445, CCDC 1936446, respectively). This data can be obtained free of charge at www.ccdc.ac.uk/data\request/cif. Specific syntheses of the molecules; additional references; and additional NMR spectra. Supplementary material 1 (PDF 9566 kb)
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1.Department of Chemistry and BiochemistryEugeneUSA
Pedroarena, J.R., Nell, B.P., Zakharov, L.N. et al. J Inorg Organomet Polym (2020) 30: 196. https://doi.org/10.1007/s10904-019-01288-9
Received 03 July 2019
First Online 21 August 2019


The purpose of this book - in an accessible way to introduce the designer with the basic principles of creating composite structures, it is applied to the amateur aircraft construction. Therefore, the book does not deal with expensive materials or complex technology.
an example of manufacturing the aircraft structure of the sandwich panels.
In addition to the diagrams and descriptions of manufacturing technology of composites, the book also contains illustrated examples of structure 5 aircraft of various types. 290 photos of the wing structure, the fuselage and tail during manufacture and assembly.


text:
You are at:Home » Columns » Minneapolis bans officers from attending training that is 'fear based'
Minneapolis Mayor Jacob Frey has banned training that is "fear based" and allegedly creates a "warrior" mentality in police officers.
Minneapolis bans officers from attending training that is 'fear based'
By Joe Vargas on April 19, 2019 Columns
Yesterday, Mayor Jacob Frey of Minneapolis announced during his annual State of the City address he would no longer allow police officers to attend "fear-based or warrior training" classes. His reason for the ban is the courses make officers overly aggressive and that's counterproductive to community policing.
https://twitter.com/Jacob_Frey/status/1119318062627459073
"Fear-based trainings violate the values at the very heart of community policing. When you're conditioned to believe that every person encountered poses a threat to your existence, you simply cannot be expected to build out meaningful relationships with those same people," Frey said in his address.
Frey, like many others, seems to have stereotyped officers into caricatures of Tackleberry from the "Police Academy" movies. His decision is based upon stereotypes and anecdotical observation and is just plain wrong.
I have attended "officer survival" training. It didn't turn me into a paranoid, trigger happy, knuckle dragger. In fact, it had quite the opposite effect. The training taught me to be more aware of my surroundings, be more deliberate about defusing encounters, and taught me how to safely engage dangerous individuals.
Cited by many in the decision is the Philando Castile shooting that occurred in 2016. A St. Anthony police officer shot Castile thinking he was going for his concealed firearm. The officer had taken a "Bulletproof Warrior" class. My personal thoughts are the officer overreacted and allowed his fear to dictate his response. That is contrary to what officer survival classes teach. You are taught to control your fear.
No research I have found shows any correlation between training and officer-involved shootings. Policy is being dictated strictly by political expediency and "what they think", rather than "what they know." I wonder if the mayor or his staff members spoke with anyone who has attended the training?
Here is some of the information Frey didn't cite in his decision. Fifty-two police officers were shot to death last year. That's not a big number given there are nearly a million law enforcement officers in the country. This is probably due to the excellent training officers receive in staying safe and alive.
There is no data that accurately tells us how many officers were shot and injured in any given year. The closest I can find is data gathered by LESMA Law Enforcement Supporters for Media Accountability. According to their data, 278 police officers were shot and injured in 2016. That's a lot of bad guys with guns shooting at the police.
There is also the fact that over 8,000 officers a year are injured by violence. The goal of the training is simple. It's to avoid dying and not getting hurt.
The day before the mayor was making his announcement, police officers in the city of Fremont, CA were ambushed by a suspect for what appears to be no reason. Quick thinking and a tactical response kept all the officers alive and the community safe.
There is also no data that tells us how many officers have been shot at and escaped injury. We don't know in any given year how many armed suspects police officers encounter and successfully take into custody without harm to anyone.
Frey believes police officers are trained to be trigger happy. Police officers are trained to stay alive. They are trained to keep others alive. They are trained to react and make split-second decisions in the most taxing of situations. It's not paranoia when the threats are real.
A department has a responsibility to evaluate training and ensure it is conducted professionally and fits the department's objectives and goals. Training decisions should be based on the realities of the job, not on political pandering. In this case I think Frey is basing his decision on perception rather than factual information.
Column: Don't wear sandals to Bakersfield Police Department's S.W.A.T school
Number of officers shot has increased 19 percent over same time last year


text:
Children of the Corn - Sight Unseen
Thread starter Steffen König
Steffen König
I was wondering what could be meant by "sight unseen" in the following paragraph:
'They were standing in a bar of dusty sunlight that fell through the lunchroom's big plate-glass window and again he had that feeling of being watched and he thought of the boy they had in their trunk, and of the high laughter of children. A phrase came to him for no reason, a legal-sounding phrase, and it began to repeat mystically in his mind: Sight unseen. Sight unseen. Sight unseen.'
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Steffen König said:
sight un·seen
[sīt ˌənˈsēn]
without the opportunity to look at the object in question beforehand:
"they bought their computers sight unseen through the mail"
without being seen:
"what other treasures remain sight unseen?"
So in the story's context it simply refers to an invisible observer? At this point of story, Burt has the feeling thatche's being watched...
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prufrock21
Let's explore the term further. Would you buy a property from Mr. D. Trump "sight unseen"?
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prufrock21 said:
No. Not after reading Ellis' American Psycho.
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jdt827
Sorry I'm so late to the party. I just finished the story. I think what he meant by Sight unseen is referring to the boy he hit. He didn't see it until he hit it. That was my take away from it.
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I think it originates from the Lithuanian movie director Larsh Syton. He had an unorthodox viewpoint which eventually became known as a 'Syton Scene'.
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mal said:
...I see what you did there.....
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Mary Strickland
Question, I have been looking back to older SK works and want to know is Children of the Corn the title of a story, included in a collection of stories, or the title of a book?
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Mary Strickland said:
Children of the Corn is a short story which was part of the Night Shift collection.
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Moderator said:
Thank you, I think. I checked out Night Shift from the library and their only copy was audio on 10 CD's. I was looking for Sometimes They Come Back which was listed as the last selection. BTW, Children of the Corn is not listed on this copy of Night Shift. I listened to CD 10, but Sometimmes They Come Back was not on it. You cannot see, touch or feel stories on audio medium and, more than anything, I wanted to sling the CD's like frisbies into the next county. I will find and buy these two stories in print. So you provided the answer I needed after all. lol
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I could look how it was translated here, but I lost the first part of Night Shift unfortunately (at one time Night Shift and Skeleton Crew came out here 'broken up' into several smaller books, Night Shift had two and Skeleton Crew three).
Amazingly they're doing yet another film. It looks like it's a prequel this time, leading up to when the parents were killed:
Children of the Corn (2020) - IMDb
Directed by Kurt Wimmer. With Elena Kampouris, Kate Moyer, Alyla Browne, Connor Burke. The film describes the events leading up to, and including, the massacre of the adults of a small town in Nebraska by their children, after the adults' irresponsibility ruins the crop and the children's future.
www.imdb.com
The longevity of this particular story in movies is incredible. I wonder why they return to it over and over again. You never hear about a big fan base for these movies, but still they must be incredibly popular.
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I'm always amazed at how close the story is to the Spanish horrorfilm 'Who can kill a Child' from 1976. It is exactly the same premise, just on a Spanish island instead of a Nebraska town. Of course in the Spanish film there is no corn, but just like in the story it's a couple that come to the deserted town and there's nothing at first, until slowly the presence of the children is revealed.
And both take place in the heat in the summer. And they both have a scene involving a church, although in the Spanish film it's not emphasized the children are killing because of religion - there is no real reason given, but actual newsreel footage of children suffering because of wars is shown at the beginning, so it is implied the children are fed up with how they have to suffer because of how adults keep fighting each other in wars. In any case it's left up mainly to your imagination, but the newsreel footage has to mean something, otherwise it wasn't put there at the start of the film.
The story was published about a year after the film premiered in Spain, but the film came out a year after the story in the US. So SK could have only seen the film if he had been in Europe when it premiered.
Who Can Kill a Child? (1976) - IMDb
Who Can Kill a Child? (1976) on IMDb: Movies, TV, Celebs, and more...
I forgot to say, as you can see in the trailer of the film a scythe is wielded by the children in 'Who can kill a Child?' too. So I think it's almost certain SK was inspired by the film, the scythe giving him the idea for the corn.
I listened to the commentary track of 'Who can kill a Child?' and Kat Ellinger, a genre expert who does many commentaries and writes interesting booklets for blu-ray releases, mentions 'Children of the Corn' and how it is very similar. There are also some differences: the children in the Spanish film are still very much children in the sense that they see it all as playing - they giggle and laugh each time they do something horrible. But both in the film and SK's story the children are extremely vicious.
Ellinger also feels 'Children of the Corn' is closer to folk horror than 'Who can kill a Child?', because there is a pagan god ('He who walks behind the rows') in it.
The Spanish film was based on this book - but very different from it:
El juego de los niños
El juego de los niños es una novela sobrecogedora que nos sumerge en una inquietante y sorprendente pesadilla, en la más apocalíptica rea...
In the book (which doesn't seem available in English) the reason for the children's behaviour is a yellow powder that has fallen from the sky. In the film it seems the children communicate by telepathy. The film is also a lot like Hitchcock's The Birds, the director of photography says: there is no direct reason given as to why it happens, but suddenly it happens. It's a sort of 'nature strikes back' idea.
And the ending of the film has a lot in common with Night of the Living Dead.


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Concord Park Trails features 13.7 miles of trail for hikers, mountain bikers and trail runners. Trails are divided into 3 sections. The main trail section (map 1) features 9.4 miles of rolling and twisting singletrack. There are 7.3 miles on the east side of the parking area with an additional 2.1 miles of trail across the drive on the west side of the parking area. The newest trail section (map 2) sits adjacent to the roundabout at the intersection of Northshore and Concord Road. These trails feature 2.6 miles of natural trail for walking, running, and mountain biking. To get to these trails, users can park at the Cove and take the 0.9-mile paved greenway from the Cove. The trailhead entrance is by the old bridge on the west end of the property. Riders are asked not to ride this trail system during or directly after inclement weather as there will be boggy sections.
Concord Park East // 10909 Northshore Dr.
There are 11.2 miles of singletrack trails for hikers, mountain bikers and trail runners. Trails are divided into 2 sections. The main trail section features 9.4 miles of rolling and twisting singletrack. There are 7.3 miles on the east side of the parking area with an additional 2.1 miles of trail across the drive on the west side of the parking area.
The Cove at Concord// 11808 S. Northshore Dr.
The newest trail section (map 2) sits adjacent to the roundabout at the intersection of Northshore and Concord Road. These trails feature 2.6 miles of natural trail for walking, running, and mountain biking. To get to these trails, users can park at the Cove and take the 0.9-mile paved greenway from the Cove. The trailhead entrance is by the old bridge on the west end of the property.


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