Inorganic Chemistry (CH415) Spring 2012

11/04/2018

Syllabus

Inorganic Chemistry (CH415) Spring 2012

Instructor:Daniel A. Smith, office Sci 316, Phone 7315 (535-7315)

Text:“Shriver and Atkins Inorganic Chemistry” 4th Ed. P. Atkins,T. Overton, J. Rourke, M. Weller, and F. Armstrong; W.H. Freeman and Company, New York, 2006.

Suggested lab texts (available on reserve in library)

A “Synthesis and Technique in Inorganic Chemistry” 3rd G. S. Girolami; T. B. Rauchfuss; R. J. Angelici; University Science Books, Mill Valley, CA, 1986.

B “Synthesis and Technique in Inorganic Chemistry” 2nd R. J. Angelici; University Science Books, Mill Valley, CA, 1986.

C “Microscale Inorganic Chemsitry: A Comprehensive Laboratory Experience” Z. Szafran; R. M. Pike; M. M. Singh; John Wiley and Sons, Inc. New York, NY, 1991.

** Indicates only one student can do the experiment at a time

DateDayChapterTopicLAB text#NSS.

Jan4W1,2Syllabus/Introduction/Atomic Structure (student responsible for material)

5RCheckin/safety/discuss NSSA

9M3Solids

11W

12RExp #13 Preparation of [Co(NH3)5Cl]2+ (2 day)A 2

13F

16MMLK day

18W5.10,6 Latimer diagrams / Physical Techniques

19Rsetup for CrCl3(THF)3 (exp 6)B

20F

23M

25W7,8Molecular Symmetry (review) / Coordination Compounds / Nomenclature

26RSynthesis of CrCl3(THF)3 (1 day) B1

27F

30M9Hydrogen

Feb1WService Learning Day

2RLinkage Isomers exp 20(2 day) (Pd and Cu)C2

6M10 Group 1

8WEXAM I (chapters 1-8)

9RExp #4 Borane-amine adduct BH3←NH2C(CH3)3 (2 day)A**1

10F

13M11 Group 2

15W12Group 13

16R

17F

20M13Group 14

22W14Group 15

23RExp #11 Metal-Metal Quadrupole Bonds (A and 1/2B)(2 days)A2

24F15Group 16

27- Mar2 M-F Midterm break

Mar5M16Group 17Halogens

7W17Group 18 Noble Gases

9F18d-block

12M

14WEXAM II (chapters 9-18)

15RSynthesis and Chromatography of Ferrocene Derivatives (2 day)B+C2

16F19d-metal electronic spectra

19M

21W20 Coordination Chemistry (reaction mechanisms)

22R

23F21d-metal organometallic chemistry

26M

28W22f-block

29R

30FGood Friday

April2M25Catalysis

5RCatalytic formation of cyclopropanes(2 day) handout - Moodle1

6F26Bioinorganic

11W23,24Solid State / Nanomaterials

12R Checkout

13FEXAM III (chapters 19-26)

16MReading Day

April18R8:00 a.m.Final Exam(ACS exam)

Assigned Reading:

The text is to be read as scheduled above. I will assume that you have read the chapter by the time I have completed lecturing on that chapter.

Class attendance:

Although class attendance will not be recorded, it is expected that you will attend class regularly.

Habitual tardiness is disrespectful of your instructor and classmates by causing frequent disruptions in the lectures and, therefore, will be inexcusable. Habitual tardiness and/or frequent absence may be reflected in a lowering of your grade.

Problems:

Problems will be assigned as the semester progresses. They are suggested problems to be worked as you study the assigned chapters. They are representative of the type of problem that may be on the hour exams.

Laboratory:

General: Each student is expected to keep a complete notebook (black, GoshenCollege notebook). Laboratory “write-ups” will consist of completing New Substance/Procedure sheets (NSS). The sheets are expected to be complete, with the exception of the spectral characterization section, which will vary for each compound prepared. The laboratory will be graded based on completeness and accuracy of the information on the New Substance/Procedure sheets.

New Substance Sheets are due two weeks after the synthesis was completed.

Spectral Characterization: Complete as much spectral characterization as you can for each of the new compounds that you synthesize. Typically at least three characterization techniques are required to confirm a compounds identity. We may not succeed in achieving this amount of characterization for all of our prepared compounds due to time and availability of techniques. Typically 1H and 13C NMR, IR, and UV/VIS should be conducted and assignments for the observed spectra should be made when possible as shown on the sample New Substance/Procedure sheet attached to this syllabus. Melting point/decomposition temperatures are encouraged but should not replace more helpful spectra when they could be obtained.

Detailed Experimental: The experimental section should be in a succinct paragraph form as on the attached sheets.

Laboratory Notebook expectations are on an attached sheet at the end of the syllabus.

Hour Exams: Three one hour exams are scheduled. Any topic covered in lecture, lab, or assigned reading prior to the exam is considered legitimate exam material. The exam will concentrate mostly on the material since the previous exam. On occasion topics from previous exams may be reexamined if, as a class, we have clearly not mastered the material on our first pass, such topics will be announced prior to the exam.

Final Exam: This will be a comprehensive exam covering the content of the entire semester. I plan to administer the ACS standardized exam.

Extra credit: Each student will be given one opportunity to fill in as much of the periodic table (first 103 elements) as possible from memory. Eachelemental symbolincorrectly located will be - 1/3 of a point with a maximum for the entire table of 30 points. You are not required to do this activity, but should note it is equivalent to two laboratories.

GradingItemnumber and valuePossible PointsPercent of

of eachtotal grade

Exams3 x 15045044%

Final1 x 20020020 %

Labs(compounds)13 x 1519519 %

weekly notebook checks12 x 1012012%

Notebook1 x 50505 %

Periodic Table1 x 3000%

Grades will be based on a straight percentage scale with minimum cutoffs being A - 93%, A-- 90%, +B - 87%,

B – 83%, -B – 80%, +C – 77%, C-73%, -C – 70%, +D – 67%, D-60%. I reserve the privilege to lower the grading scale at the end of the semester. To assure a particular letter grade use the above scale. For each NSS not completed the final grade will be lowered by a full letter grade (10 percentage points) in addition to the 15 points from missing the assignment. The course grade is not intended to be a wage, neither is the grade intended to reflect how hard you have worked. They are intended to be a measure of your ability to collect, process and discuss data as a mature scientist relative to other members of your class and previous classes.

Academic Integrity

Plagiarism is a serious offense in any academic community. In the laboratory it is particularly serious. Academic dishonesty in this laboratory course (ie. sharing of lab data, spectra or write ups or using notebooks, reports, data or spectra from a previous year) will result in a minimum penalty of lowering the course grade by two letter grades. In addition, a letter will be sent to the Associate Academic Dean to be placed in the offender’s permanent record. Additional consequences are possible as outlined in the student handbook.

Academic Support

GoshenCollege wants to help all students be as academically successful as possible. If you have a disability and require accommodations, please contact the instructor or the Director of the Academic Support Center, Lois Martin, early in the semester so that your learning needs may be appropriately met. In order to receive accommodations, documentation concerning your disability must be on file with the AcademicSupportCenter, KU004, x7576, . All information will be held in the strictest confidence. The AcademicSupportCenter offers tutoring and writing assistance for all students. For further information please see

Reading Room

You have access to the Chemistry Reading Room using your Goshen College ID. You may either swipe your ID card or type in your ID number to gain access to this room whenever the building is open. You are not to allow any other person to enter the room unless they are a Goshen College student. Do not prop the door open – it is to remain locked.

Laboratory Notebook Expectations

Your notebook will be set up as follows:

Each page will contain:

top right: page number, date, and signature

top center: title of experiment

top left: page continued from

bottom right: page experiment continues on

Each experimental write-up will take this format:

Reaction summary or Brief outline of expected procedure if procedure is not a reaction

Safety precautions: experimental and chemical hazards (check MSDS sheets each reagent used!!)

2A+BC

10 g15 g solventexpected massIf reagent is a liquid report

20g/mole60 g/moleactual massvolume on top line then density

0.5 mole0.25 mole% yieldfollowed by information shown

Safety infosafety infosafety info

Reference the procedure

The above sections will be completed before entering the laboratory !

Detailed experimental written as the experiment is conducted. This should be in sufficient detail to allow another chemist to duplicate your experiment exactly!

The above section will be completed while in the laboratory !

Calculations % yield, rate constants, etc.

Discussion In paragraph form, clearly and concisely report and discuss your findings (include error limits), compare your results to any literature available, show equations and/or calculations, compare, contrast and comment on methods used.)

Graphs and Tables (Include: Title, Labels on both axes, drawn in ink, they should be of high quality graphics if drawn on a computer, use an 8 1/2-11 inch page for each one.)

Copies of data and spectra (Originals are permanently fixed in your notebook)

Concluding paragraph (Summary of results in 4-6 sentences. What are the major points of your work. Again the findings and uncertainties will be clearly stated.)

References (list a bibliography for all references which you referred to during the lab or while writing your discussion). Examine several recent JACS communications and articles to familiarize yourself with style and reference requirements. References are to be in the ACS accepted format, for articles this is typically:

Lastname1, FI1.; Lastname2, FI2. Journ. Abbr.Year, Volume, firstpage-lastpage.

and for texts:

Authors (Lastname1, FI1.; Lastname2, FI2.) title; Editor (Lastname1, FI1.; Lastname2, FI2., Ed.); Publisher, city, state (or country), Year; Vol., chapter, page(s) (p or pp.).

General notes about your notebook:

1) Include a table of contents on the first page (or two).

2) Do not skip pages intending to fill them in later. If you begin a second experiment before you finish writing up the first experiment, which is expected, continue on the next available page. This is why each page will say continued on/from.

3) If you make a mistake in calculations or discussion/reasoning a single line through the text or data (or an X if the entire page is in error) is sufficient. The text and data should still be legible in case at a later time you realize it was correct.

4) Spelling and grammar are not of primary concern in the notebook although it should be clearly legible and discernible.

5) You may include under discussion ways to improve the experimental accuracy.

6) The use of spread sheets (Excel) are encouraged. Printouts from a spread sheet may be fastened permanently to your notebook to facilitate efficient use of time and avoid coping errors.

7) Write only on the right hand pages. Use the left hand pages for scratch and storing spectra, graphs, excel printouts, etc.

8) No scratch paper should be in the lab, record all observations directly into your notebook!!!

9) All spectra and supporting documents should be permanently fastened to the notebook. Loose pages will be removed. Remember this is the only permanent record of the experiment!

New Substance / Procedure

Submitted by: Helmut Werner

Notebook reference:from literatureDate:April 16,1996

Preparation/Analysis/Kinetics of (give code name(s) and approved nomenclature):(2 pt)

[RuCl2(=C=CHPh)(PiPr3)2] trans,trans-dichlorobis(triisopropylphosphine)phenylvinylideneruthenium(II)

Reaction (Give structural formulas and molecular masses):% yield(1 pt)

[RuH2Cl2(PiPr3)2] + PhCCH CH2Cl2 [RuCl2(=C=CHPh)(PiPr3)2] 66 %

494 g/mole 102 g/mole 594 g/mole

Sketch of molecule:(1 pt)

H Ph

C PiPr3

Cl Ru Cl

PiPr3

Literature References:(1 pt)

Grunwald, C.; Gevert, O.; Wolf, J.; Gonzalez-Herrero, P.; Werner, H.; Organometallics1996, 15, 1960-1962.

RuCl2(C8H12) Albers, M. O.; Singleton, E.; Yates, J. E. Inorg. Synth.1989, 26, 253.

Sources of materials:(1 pt)

Not statedassumed to be purchased when not referenced in above article.

Submitted by: Helmut Werner

Notebook reference:from literatureDate:April 16,1996

Preparation/Analysis/Kinetics of (give code name(s) and approved nomenclature):

[RuCl2(=C=CHPh)(PiPr3)2] trans,trans-dichlorobis(triisopropylphosphine)phenylvinylideneruthenium(II)

Spectral Characterization:(3 pt)

1H NMR (solvent)13C NMR (solvent)

(400 MHz, C6D6)(100.6 MHz, C6D6)

7.12 (m, 5H, C6H5)341.11 (t, Ru=C)

4.71 (t, 1H, =CHPh)133.76 (t, ipso-C of C6H5)

2.79 (m, 6H, PCH(CH3)2)128.53

1.29 (dt, 36H, PCH(CH3)2125.59 (all s, C6H5)

124.37

109.34 (t, =CHPh)

23.66 (t, PCH(CH3)2)

20.11 (s, PCH(CH3)2)

31P NMR (162 MHz, C6D6)

UV/VIS (solvent)29.0 (s)

IR (method/solvent)

(KBr) (C=C) 1600 cm-1

Melting point: 97 C dec

Mass spectrum:

Elemental analysis(company): Calc. C 52.52 H 8.14

Exp. 52.85 7.86

X-Ray Structure:

Other:

Submitted by: Helmut Werner

Notebook reference:from literatureDate:April 16,1996

Preparation/Analysis/Kinetics of (give code name(s) and approved nomenclature):

[RuCl2(=C=CHPh)(PiPr3)2] trans,trans-dichlorobis(triisopropylphosphine)phenylvinylideneruthenium(II)

Special Precautions and Safety Data:(1 pt)

Air sensitive/Dry solvents?

Detailed experimental:(5 pt)

A solution of [RuH2Cl2(PiPr3)2] (142 mg, 0.29 mmol) in 7 ml of CH2Cl2 was treated with phenyl acetylene (63 L, 0.57 mmol) and stirred for 5 min. at room temperature. After the solvent was removed, the oily residue was dissolved in 5 ml of benzene and phenylacetylene (30 l, 0.27 mmol) was added. The reaction mixture was heated for 10 min to 80 C, and upon being cooled to 25 C, the solution was brought to dryness in vacuo. Recrystillization from methanol gave 113 mg of a brown microcrystaline solid (66 %).