PDF
Instructor
Teaching Assistant
Uma P. Mallik , R 306, Research Bldg., umty8@umsl.edu
Course Description
Prerequisites: CHEM 3333, CHEM 4412 and CHEM 3643, (CHEM 3643 may be taken concurrently). The more sophisticated techniques of physical and analytical chemistry will be used to study inorganic compounds and their reactions. One hour of lecture and four and one-half hours of laboratory per week. Not for graduate credit. CHEM 4433 is a two credit hour lecture/laboratory course. See: http://www.umsl.edu/bulletin/as/chemistry.html . This is an advanced laboratory course. It is assumed that you have previously and satisfactorily mastered concepts, techniques, and applications in prior coursework (e.g. CHEM 2612, 2622, 3412, 4412) concerning NMR, Infrared, UV-vis spectroscopy, organic synthesis and mechanisms, and inorganic chemistry theory and applications. CHEM 4433 is a two credit hour writing intensive laboratory course that introduces the student to inorganic synthetic techniques, magnetism, and structural determination techniques and methods. In this course you will (1) review and apply inorganic chemistry principles and physical characterization techniques, (2) perform laboratory experiments, and (3) write and complete formal J. Am. Chem. Soc.-style reports (in manuscript format). As a general rule, at least 6 hours per week should be devoted to studying concepts introduced in class and the textbook; homework problem sets are considered in addition to this suggestion and will generally take 2-4 hours if these concepts are understood. Working in groups and scheduling office hours may also aid students in these efforts. Report writing times will depend on the individual but expect to take at least 5-6 hours for the construction of each report. If work, other courses, and/or other responsibilities will not allow for these time investments, please see the instructor as soon as possibleto discuss possible options. The reports will demonstrate your understanding of basic laboratory synthesis, spectroscopy, data interpretation, and inorganic chemistry. The most important outcomes of your efforts are to know the basics of inorganic chemistry, think critically about a particular reaction pathway or set of data, and predict/propose likely outcomes and/or reasons for the observed behavior.
Prerequisites: CHEM 3333, CHEM 4412 and CHEM 3643, (CHEM 3643 may be taken concurrently). The more sophisticated techniques of physical and analytical chemistry will be used to study inorganic compounds and their reactions. One hour of lecture and four and one-half hours of laboratory per week. Not for graduate credit. CHEM 4433 is a two credit hour lecture/laboratory course. See: http://www.umsl.edu/bulletin/as/chemistry.html .
This is an advanced laboratory course. It is assumed that you have previously and satisfactorily mastered concepts, techniques, and applications in prior coursework (e.g. CHEM 2612, 2622, 3412, 4412) concerning NMR, Infrared, UV-vis spectroscopy, organic synthesis and mechanisms, and inorganic chemistry theory and applications. CHEM 4433 is a two credit hour writing intensive laboratory course that introduces the student to inorganic synthetic techniques, magnetism, and structural determination techniques and methods.
In this course you will (1) review and apply inorganic chemistry principles and physical characterization techniques, (2) perform laboratory experiments, and (3) write and complete formal J. Am. Chem. Soc.-style reports (in manuscript format). As a general rule, at least 6 hours per week should be devoted to studying concepts introduced in class and the textbook; homework problem sets are considered in addition to this suggestion and will generally take 2-4 hours if these concepts are understood. Working in groups and scheduling office hours may also aid students in these efforts. Report writing times will depend on the individual but expect to take at least 5-6 hours for the construction of each report. If work, other courses, and/or other responsibilities will not allow for these time investments, please see the instructor as soon as possibleto discuss possible options.
The reports will demonstrate your understanding of basic laboratory synthesis, spectroscopy, data interpretation, and inorganic chemistry. The most important outcomes of your efforts are to know the basics of inorganic chemistry, think critically about a particular reaction pathway or set of data, and predict/propose likely outcomes and/or reasons for the observed behavior.
Course Text
G. S. Girolami, T. B. Rauchfuss, R. J. Angelici Synthesis and Technique in Inorganic Chemistry, 3rd Ed.
Supplementary Texts
Useful Course Information/Helpful Links
On these websites you will find descriptions of the course syllabus, laboratory rules & safety, instructions, and report templates. For additional assistance with writing assignments also consult (http://pubs.acs.org/journal/jacsat/), course instructor, and the UMSL Writing Lab.
Grading Distribution
5 x 100 (Exp. 2-6)
1 x 200 (Exp. 7)
Course Grade = [Acquired Points/Total Possible Points] x 100%: 100% < A < 90% < B < 80% < C < 70% < D < 60% < E
Course Grade = [Acquired Points/Total Possible Points] x 100%:
100% < A < 90% < B < 80% < C < 70% < D < 60% < E
Absences
University of Missouri SystemExcused Absences
There are no “make up” laboratory sections or times. Participation in scheduled University events will require you to work diligently in a time efficient manner within the allotted or remaining laboratory time during the semester. Absences due to an excused illness will require similar measures on your part.
Students with Disabilities
Students are required to request accommodation services though the Disability Access Services office [144 MSC, (314) 516-6554]. Students that may require special accommodations should first, register with Disability Access Services (DAS), and second, meet with the instructor in-person; the notification memo generated by DAS should be provided to the instructor as soon as it becomes available. For more information please consult the University of Missouri Collected Rules and Regulations [240.040] or the following links: http://www.umsl.edu/services/disabled/aidpolicy.htm http://www.umsl.edu/services/disabled/testingacdm.html
Students are required to request accommodation services though the Disability Access Services office [144 MSC, (314) 516-6554]. Students that may require special accommodations should first, register with Disability Access Services (DAS), and second, meet with the instructor in-person; the notification memo generated by DAS should be provided to the instructor as soon as it becomes available. For more information please consult the University of Missouri Collected Rules and Regulations [240.040] or the following links:
Academic Dishonesty
The penalties for academic dishonesty are severe and may lead to earning a zero on an assignment, failure of the course, and expulsion from the University. The UMSL College of Arts & Sciences requires that you understand and acknowledge what constitutes academic honesty and dishonesty. This document is available online (via course website and MyGateway) and signed a copy of this document (required) will be kept on file. For further information concerning what constitutes plagiarism, academic dishonesty, and misconduct please consult the University of Missouri Collected Rules and Regulations [200.010] or Student Conduct Codes via the following website links. UMSL Arts & Sciences Academic Honesty Statement: via MyGateway or via link. http://www.umsystem.edu/ums/departments/gc/rules/programs/200/010.shtml http://www.umsl.edu/studentlife/dsa/student_planner/policies/conductcode.html
The penalties for academic dishonesty are severe and may lead to earning a zero on an assignment, failure of the course, and expulsion from the University. The UMSL College of Arts & Sciences requires that you understand and acknowledge what constitutes academic honesty and dishonesty. This document is available online (via course website and MyGateway) and signed a copy of this document (required) will be kept on file.
For further information concerning what constitutes plagiarism, academic dishonesty, and misconduct please consult the University of Missouri Collected Rules and Regulations [200.010] or Student Conduct Codes via the following website links.
UMSL Arts & Sciences Academic Honesty Statement: via MyGateway or via link.
(1) Lecture Class attendance and participation are critical to success. Regular attendance will help you to learn the course material and allow the opportunity to ask questions as they may arise. It is your responsibility to keep up with the assigned reading, homework, and lecture discussions. To assist in mastery of the course material I also strongly encourage you to form study groups early in the semester. Active participation by all during class will help everyone to learn the material as a group and often decreases individual study time necessary outside of class (yes, really). As a courtesy to others enrolled in the course electronic device use (e.g. cell phones, iPods, and computers) is not allowed during class; all should be turned off or their ringers disabled and safely stored. Devices necessary for participating in the course (e.g. hearing aids, etc.) are excluded from this rule. Please refer to the University of Missouri Collected Rules and Regulations [200.010] for more information. http://www.umsystem.edu/ums/departments/gc/rules/programs/200/010.shtml (2) Homework Problem Sets Two homework sets will be assigned during the semester. These assignments are designed so that you practice and apply knowledge acquired during class and readings outside of class. Some assignments will require more time than others. Expect to spend at least 2 hours per assignment. (3) Laboratory Safety and Attire Safety is of utmost importance in the laboratory. Shorts, dresses, tank tops, and open-toed shoes are not permitted within the CHEM 4433 laboratory. Laboratory coats and/or aprons are not required but are highly recommended. Food and drink are also forbidden. At all times goggles will be worn within the lab and failure to do so will result in one of the following: (first offense) a verbal warning, (second offense) a 5% reduction of the laboratory technique/safety grade, and (3) expulsion from the laboratory; no make-up time will be allowed. Subsequent offenses will require discussions with the Instructor, student, and Chemistry Department chairperson to decide the appropriate measures to be taken. (4) Experiments, Notebook, and Reports Scheduled Experiments Seven laboratory experiments are scheduled. These experiments are: Introduction to Laboratory Glassblowing Determination of Do in Cr(III) Complexes (Handout) Optical Resolution of Co(en)33+ (Girolami 14) The Oxidation States of Tin (Girolami 7 & Handout: Tin Iodide) Binary Transition Metal p-Toluenesulfonates (Handout) The Metal-Arene Complex [1,3,5-C6H3(CH3)3]Mo(CO)3 (Girolami 16) Independent Project (below) Each experiment should be easily completed within one to three scheduled 4.5 hour laboratory sections. Additional information (experimental modifications and procedures) will be provided later in the semester by the instructor online via MyGateway and the course website. Independent Projects Each student will choose from one of the Independent Projects below. This experiment will constitute your seventh laboratory experiment. Metal-Metal Quadrupole Bonds (#11 Girolami) The Paramagnetic Complex Mn(acac)3 (#12 Girolami) Metal Dithiolenes and the Use of Quaternary Ammonium Salts (#15 Girolami) Organoiron Chemistry: (C5H5)Fe2(CO)4 and (C5H5)Fe(CO)2CH3 (#17 Girolami) Magnetic Molecule-Based Magnets: CrII2[CrII(CN)6]nH2O (Handout) Superconducting YBa2Cu3O7 (#1 Girolami) Cyanometalate Complexes and Magnetic Tetranuclear Complexes (Handout) Laboratory Notebook A laboratory notebook is also required. Written reports are not an appropriate substitute for an accurate and complete notebook. Appropriate procedures, quantities of reagents, and recorded information are to be kept in you notebook. No laboratory manuals are allowed in the lab and all experimental information and recorded data will be copied to your laboratory notebook. Upon completion of the experiment carbon copies of your notebook pages (stapled) are to be submitted to your teaching assistant before beginning the next experiment. Failure to follow these guidelines will result in a 10% reduction of your report grade for each experiment. Helpful hints for constructing and using a laboratory notebook are provided on the course website. Report Construction All laboratory reports will adhere to the Journal of the American Chemical Society format for Full Manuscripts. You will submit reports on Experiments 2-7 for credit. This is a different format than what you may have utilized in previous Chemistry or Science laboratory classes. Electronic templates will be provided for each written report. Your laboratory reports (6 total) will generally consist of 12 basic sections: (1) Title, Authors, and Affiliation . Describes report contents succinctly, who did the work (you), and where work performed (Department of Chemistry & Biochemistry, University of Missouri-St. Louis). (2) Abstract . Briefly describes what experiment you did and briefly summarizes data and conclusions. A well-written abstract summarizes your report in a ~5-20 short choppy statements. (3) Introduction [a.k.a. what others have previously reported; ~1.5-2 pages]. This is not a summary of the laboratory manual introduction. Literature citations (not Websites) in proper format should also be present. Key points of the experiment appear here and often dictate differences A, B, and C grades. This often can be prepared in advance of the laboratory experiment. (4) Motivation [a.k.a. why other than a grade are you writing this document or why should we care?)]. This is again not a summary of the laboratory manual introduction (~1-2 paragraphs). Include as a portion of the Introduction section. Literature citations (not websites) in proper format should also be present. (5) Experimental/Physical Methods . This described what purification techniques for reagents, sources, prior literature synthetic details, and instrumentation (model number and any modifications) was used to prepare/characterize your reaction products. (~1-3 paragraphs, abstract style). Literature citations (not websites) in proper format should also be present. (6) Experimental. Describes the reagent quantities, times, temperatures, and pressures (etc.) used during experiment. Should be accurate and complete so that the experiment may be repeated by another. Yields and additional analysis data must also be present in short format. Use neutral past tense (i.e. no I or we). (7) Results and Discussion . This section compares your research findings to the primary research literature (i.e. not website or those in lab manual). You should describe what was done, interpret and report your data, and compare your data/conclusions to the primary literature (e.g. published manuscript). Literature citations (not websites) in proper format should also support your claims. (~2-20 pages; judgment call). The length of this section depends on the experimental data and complexity of experiment. (8) Figures, Tables, and Schemes . These should include experimental data plots (spectra, structures, etc.) or clearly indicate non-trivial chemical transformations in a graphical format. Acid-base neutralization, salt elimination, distillation apparatus, Schlenk line design, etc. are not useful. For examples consult several manuscripts that appear in the Journal of the American Chemical Society. (9) Conclusions . You should briefly describe why you performed the experiment, what conclusions were drawn, how they agree with or differ from literature reports, and propose a new avenue for study (a.k.a. future directions). This section will be ~ 1-2 paragraphs in length and is not the same as an abstract. (10) Acknowledgments . You should thank staff, faculty, and students who assisted with data collection, analysis, or experimental issues. Access to facilities outside of the laboratory and their funding sources should also be mentioned. (11) References. Primary literature citations (minimum = 20) that are used to support claims and assignments contained within the written report. Websites are not allowable sources for citations or information. The references must contain 75% original citations (i.e. other than those described in the laboratory handout or manual). The presence of online citations will result in a grade of zero and the report will be returned. Note: Must use J. Am. Chem. Soc. format. See: http://pubs.acs.org/journal/jacsat (12) Supporting Information . Includes trivial calculations, Figures, and any additional data that does not appear in the manuscript text. Report Submission All students are required to submit their reports (6 total) in PDF (last name_report number.pdf) format as an attached document in a single E-mail to holmesst@umsl.edu . Reports that are deemed too large by E-mail servers (e.g. Hotmail) will require reduction of Figures and/or Schemes data size; submissions via UMSL E-mail servers should not experience this problem. In addition, a complete and legible printed paper copy is to be submitted prior to or on the report due date (Wed. 5:30 PM). If you do not own a copy of Microsoft Word or Adobe Acrobat, this work can be performed within UMSL Chemistry & Biochemistry Computer Lab, 232 Benton Hall). Reports submitted after class are considered as “late” and are subject to a 10% penalty immediately. Each subsequent day (5 PM) is assessed an additional 10% penalty. Reports submitted two or more days (≥ 48 hours) after the due date will not be graded and a grade of “0, zero” will be assigned. Report Grade Assignment Report grading will adhere to the following weighting scheme. Abstract Introduction Results & Discussion Experimental References Notebook Spectra Sample Appearance & Labeling 5 20 20 10 5 10 10 20
(1) Lecture
Class attendance and participation are critical to success. Regular attendance will help you to learn the course material and allow the opportunity to ask questions as they may arise. It is your responsibility to keep up with the assigned reading, homework, and lecture discussions. To assist in mastery of the course material I also strongly encourage you to form study groups early in the semester. Active participation by all during class will help everyone to learn the material as a group and often decreases individual study time necessary outside of class (yes, really). As a courtesy to others enrolled in the course electronic device use (e.g. cell phones, iPods, and computers) is not allowed during class; all should be turned off or their ringers disabled and safely stored. Devices necessary for participating in the course (e.g. hearing aids, etc.) are excluded from this rule. Please refer to the University of Missouri Collected Rules and Regulations [200.010] for more information. http://www.umsystem.edu/ums/departments/gc/rules/programs/200/010.shtml
Class attendance and participation are critical to success. Regular attendance will help you to learn the course material and allow the opportunity to ask questions as they may arise. It is your responsibility to keep up with the assigned reading, homework, and lecture discussions. To assist in mastery of the course material I also strongly encourage you to form study groups early in the semester. Active participation by all during class will help everyone to learn the material as a group and often decreases individual study time necessary outside of class (yes, really). As a courtesy to others enrolled in the course electronic device use (e.g. cell phones, iPods, and computers) is not allowed during class; all should be turned off or their ringers disabled and safely stored. Devices necessary for participating in the course (e.g. hearing aids, etc.) are excluded from this rule. Please refer to the University of Missouri Collected Rules and Regulations [200.010] for more information.
http://www.umsystem.edu/ums/departments/gc/rules/programs/200/010.shtml
(2) Homework Problem Sets
Two homework sets will be assigned during the semester. These assignments are designed so that you practice and apply knowledge acquired during class and readings outside of class. Some assignments will require more time than others. Expect to spend at least 2 hours per assignment.
(3) Laboratory
Safety and Attire Safety is of utmost importance in the laboratory. Shorts, dresses, tank tops, and open-toed shoes are not permitted within the CHEM 4433 laboratory. Laboratory coats and/or aprons are not required but are highly recommended. Food and drink are also forbidden. At all times goggles will be worn within the lab and failure to do so will result in one of the following: (first offense) a verbal warning, (second offense) a 5% reduction of the laboratory technique/safety grade, and (3) expulsion from the laboratory; no make-up time will be allowed. Subsequent offenses will require discussions with the Instructor, student, and Chemistry Department chairperson to decide the appropriate measures to be taken.
Safety and Attire
Safety is of utmost importance in the laboratory. Shorts, dresses, tank tops, and open-toed shoes are not permitted within the CHEM 4433 laboratory. Laboratory coats and/or aprons are not required but are highly recommended. Food and drink are also forbidden. At all times goggles will be worn within the lab and failure to do so will result in one of the following: (first offense) a verbal warning, (second offense) a 5% reduction of the laboratory technique/safety grade, and (3) expulsion from the laboratory; no make-up time will be allowed. Subsequent offenses will require discussions with the Instructor, student, and Chemistry Department chairperson to decide the appropriate measures to be taken.
(4) Experiments, Notebook, and Reports
Scheduled Experiments Seven laboratory experiments are scheduled. These experiments are: Introduction to Laboratory Glassblowing Determination of Do in Cr(III) Complexes (Handout) Optical Resolution of Co(en)33+ (Girolami 14) The Oxidation States of Tin (Girolami 7 & Handout: Tin Iodide) Binary Transition Metal p-Toluenesulfonates (Handout) The Metal-Arene Complex [1,3,5-C6H3(CH3)3]Mo(CO)3 (Girolami 16) Independent Project (below) Each experiment should be easily completed within one to three scheduled 4.5 hour laboratory sections. Additional information (experimental modifications and procedures) will be provided later in the semester by the instructor online via MyGateway and the course website. Independent Projects Each student will choose from one of the Independent Projects below. This experiment will constitute your seventh laboratory experiment. Metal-Metal Quadrupole Bonds (#11 Girolami) The Paramagnetic Complex Mn(acac)3 (#12 Girolami) Metal Dithiolenes and the Use of Quaternary Ammonium Salts (#15 Girolami) Organoiron Chemistry: (C5H5)Fe2(CO)4 and (C5H5)Fe(CO)2CH3 (#17 Girolami) Magnetic Molecule-Based Magnets: CrII2[CrII(CN)6]nH2O (Handout) Superconducting YBa2Cu3O7 (#1 Girolami) Cyanometalate Complexes and Magnetic Tetranuclear Complexes (Handout) Laboratory Notebook A laboratory notebook is also required. Written reports are not an appropriate substitute for an accurate and complete notebook. Appropriate procedures, quantities of reagents, and recorded information are to be kept in you notebook. No laboratory manuals are allowed in the lab and all experimental information and recorded data will be copied to your laboratory notebook. Upon completion of the experiment carbon copies of your notebook pages (stapled) are to be submitted to your teaching assistant before beginning the next experiment. Failure to follow these guidelines will result in a 10% reduction of your report grade for each experiment. Helpful hints for constructing and using a laboratory notebook are provided on the course website. Report Construction All laboratory reports will adhere to the Journal of the American Chemical Society format for Full Manuscripts. You will submit reports on Experiments 2-7 for credit. This is a different format than what you may have utilized in previous Chemistry or Science laboratory classes. Electronic templates will be provided for each written report. Your laboratory reports (6 total) will generally consist of 12 basic sections: (1) Title, Authors, and Affiliation . Describes report contents succinctly, who did the work (you), and where work performed (Department of Chemistry & Biochemistry, University of Missouri-St. Louis). (2) Abstract . Briefly describes what experiment you did and briefly summarizes data and conclusions. A well-written abstract summarizes your report in a ~5-20 short choppy statements. (3) Introduction [a.k.a. what others have previously reported; ~1.5-2 pages]. This is not a summary of the laboratory manual introduction. Literature citations (not Websites) in proper format should also be present. Key points of the experiment appear here and often dictate differences A, B, and C grades. This often can be prepared in advance of the laboratory experiment. (4) Motivation [a.k.a. why other than a grade are you writing this document or why should we care?)]. This is again not a summary of the laboratory manual introduction (~1-2 paragraphs). Include as a portion of the Introduction section. Literature citations (not websites) in proper format should also be present. (5) Experimental/Physical Methods . This described what purification techniques for reagents, sources, prior literature synthetic details, and instrumentation (model number and any modifications) was used to prepare/characterize your reaction products. (~1-3 paragraphs, abstract style). Literature citations (not websites) in proper format should also be present. (6) Experimental. Describes the reagent quantities, times, temperatures, and pressures (etc.) used during experiment. Should be accurate and complete so that the experiment may be repeated by another. Yields and additional analysis data must also be present in short format. Use neutral past tense (i.e. no I or we). (7) Results and Discussion . This section compares your research findings to the primary research literature (i.e. not website or those in lab manual). You should describe what was done, interpret and report your data, and compare your data/conclusions to the primary literature (e.g. published manuscript). Literature citations (not websites) in proper format should also support your claims. (~2-20 pages; judgment call). The length of this section depends on the experimental data and complexity of experiment. (8) Figures, Tables, and Schemes . These should include experimental data plots (spectra, structures, etc.) or clearly indicate non-trivial chemical transformations in a graphical format. Acid-base neutralization, salt elimination, distillation apparatus, Schlenk line design, etc. are not useful. For examples consult several manuscripts that appear in the Journal of the American Chemical Society. (9) Conclusions . You should briefly describe why you performed the experiment, what conclusions were drawn, how they agree with or differ from literature reports, and propose a new avenue for study (a.k.a. future directions). This section will be ~ 1-2 paragraphs in length and is not the same as an abstract. (10) Acknowledgments . You should thank staff, faculty, and students who assisted with data collection, analysis, or experimental issues. Access to facilities outside of the laboratory and their funding sources should also be mentioned. (11) References. Primary literature citations (minimum = 20) that are used to support claims and assignments contained within the written report. Websites are not allowable sources for citations or information. The references must contain 75% original citations (i.e. other than those described in the laboratory handout or manual). The presence of online citations will result in a grade of zero and the report will be returned. Note: Must use J. Am. Chem. Soc. format. See: http://pubs.acs.org/journal/jacsat (12) Supporting Information . Includes trivial calculations, Figures, and any additional data that does not appear in the manuscript text. Report Submission All students are required to submit their reports (6 total) in PDF (last name_report number.pdf) format as an attached document in a single E-mail to holmesst@umsl.edu . Reports that are deemed too large by E-mail servers (e.g. Hotmail) will require reduction of Figures and/or Schemes data size; submissions via UMSL E-mail servers should not experience this problem. In addition, a complete and legible printed paper copy is to be submitted prior to or on the report due date (Wed. 5:30 PM). If you do not own a copy of Microsoft Word or Adobe Acrobat, this work can be performed within UMSL Chemistry & Biochemistry Computer Lab, 232 Benton Hall). Reports submitted after class are considered as “late” and are subject to a 10% penalty immediately. Each subsequent day (5 PM) is assessed an additional 10% penalty. Reports submitted two or more days (≥ 48 hours) after the due date will not be graded and a grade of “0, zero” will be assigned. Report Grade Assignment Report grading will adhere to the following weighting scheme.
Scheduled Experiments
Seven laboratory experiments are scheduled. These experiments are: Introduction to Laboratory Glassblowing Determination of Do in Cr(III) Complexes (Handout) Optical Resolution of Co(en)33+ (Girolami 14) The Oxidation States of Tin (Girolami 7 & Handout: Tin Iodide) Binary Transition Metal p-Toluenesulfonates (Handout) The Metal-Arene Complex [1,3,5-C6H3(CH3)3]Mo(CO)3 (Girolami 16) Independent Project (below) Each experiment should be easily completed within one to three scheduled 4.5 hour laboratory sections. Additional information (experimental modifications and procedures) will be provided later in the semester by the instructor online via MyGateway and the course website.
Seven laboratory experiments are scheduled. These experiments are:
Each experiment should be easily completed within one to three scheduled 4.5 hour laboratory sections. Additional information (experimental modifications and procedures) will be provided later in the semester by the instructor online via MyGateway and the course website.
Independent Projects
Each student will choose from one of the Independent Projects below. This experiment will constitute your seventh laboratory experiment. Metal-Metal Quadrupole Bonds (#11 Girolami) The Paramagnetic Complex Mn(acac)3 (#12 Girolami) Metal Dithiolenes and the Use of Quaternary Ammonium Salts (#15 Girolami) Organoiron Chemistry: (C5H5)Fe2(CO)4 and (C5H5)Fe(CO)2CH3 (#17 Girolami) Magnetic Molecule-Based Magnets: CrII2[CrII(CN)6]nH2O (Handout) Superconducting YBa2Cu3O7 (#1 Girolami) Cyanometalate Complexes and Magnetic Tetranuclear Complexes (Handout)
Each student will choose from one of the Independent Projects below. This experiment will constitute your seventh laboratory experiment.
Laboratory Notebook
A laboratory notebook is also required. Written reports are not an appropriate substitute for an accurate and complete notebook. Appropriate procedures, quantities of reagents, and recorded information are to be kept in you notebook. No laboratory manuals are allowed in the lab and all experimental information and recorded data will be copied to your laboratory notebook. Upon completion of the experiment carbon copies of your notebook pages (stapled) are to be submitted to your teaching assistant before beginning the next experiment. Failure to follow these guidelines will result in a 10% reduction of your report grade for each experiment. Helpful hints for constructing and using a laboratory notebook are provided on the course website.
Report Construction
All laboratory reports will adhere to the Journal of the American Chemical Society format for Full Manuscripts. You will submit reports on Experiments 2-7 for credit. This is a different format than what you may have utilized in previous Chemistry or Science laboratory classes. Electronic templates will be provided for each written report.
Your laboratory reports (6 total) will generally consist of 12 basic sections:
(1) Title, Authors, and Affiliation . Describes report contents succinctly, who did the work (you), and where work performed (Department of Chemistry & Biochemistry, University of Missouri-St. Louis). (2) Abstract . Briefly describes what experiment you did and briefly summarizes data and conclusions. A well-written abstract summarizes your report in a ~5-20 short choppy statements. (3) Introduction [a.k.a. what others have previously reported; ~1.5-2 pages]. This is not a summary of the laboratory manual introduction. Literature citations (not Websites) in proper format should also be present. Key points of the experiment appear here and often dictate differences A, B, and C grades. This often can be prepared in advance of the laboratory experiment. (4) Motivation [a.k.a. why other than a grade are you writing this document or why should we care?)]. This is again not a summary of the laboratory manual introduction (~1-2 paragraphs). Include as a portion of the Introduction section. Literature citations (not websites) in proper format should also be present. (5) Experimental/Physical Methods . This described what purification techniques for reagents, sources, prior literature synthetic details, and instrumentation (model number and any modifications) was used to prepare/characterize your reaction products. (~1-3 paragraphs, abstract style). Literature citations (not websites) in proper format should also be present. (6) Experimental. Describes the reagent quantities, times, temperatures, and pressures (etc.) used during experiment. Should be accurate and complete so that the experiment may be repeated by another. Yields and additional analysis data must also be present in short format. Use neutral past tense (i.e. no I or we). (7) Results and Discussion . This section compares your research findings to the primary research literature (i.e. not website or those in lab manual). You should describe what was done, interpret and report your data, and compare your data/conclusions to the primary literature (e.g. published manuscript). Literature citations (not websites) in proper format should also support your claims. (~2-20 pages; judgment call). The length of this section depends on the experimental data and complexity of experiment. (8) Figures, Tables, and Schemes . These should include experimental data plots (spectra, structures, etc.) or clearly indicate non-trivial chemical transformations in a graphical format. Acid-base neutralization, salt elimination, distillation apparatus, Schlenk line design, etc. are not useful. For examples consult several manuscripts that appear in the Journal of the American Chemical Society. (9) Conclusions . You should briefly describe why you performed the experiment, what conclusions were drawn, how they agree with or differ from literature reports, and propose a new avenue for study (a.k.a. future directions). This section will be ~ 1-2 paragraphs in length and is not the same as an abstract. (10) Acknowledgments . You should thank staff, faculty, and students who assisted with data collection, analysis, or experimental issues. Access to facilities outside of the laboratory and their funding sources should also be mentioned. (11) References. Primary literature citations (minimum = 20) that are used to support claims and assignments contained within the written report. Websites are not allowable sources for citations or information. The references must contain 75% original citations (i.e. other than those described in the laboratory handout or manual). The presence of online citations will result in a grade of zero and the report will be returned. Note: Must use J. Am. Chem. Soc. format. See: http://pubs.acs.org/journal/jacsat (12) Supporting Information . Includes trivial calculations, Figures, and any additional data that does not appear in the manuscript text.
(1) Title, Authors, and Affiliation . Describes report contents succinctly, who did the work (you), and where work performed (Department of Chemistry & Biochemistry, University of Missouri-St. Louis).
(2) Abstract . Briefly describes what experiment you did and briefly summarizes data and conclusions. A well-written abstract summarizes your report in a ~5-20 short choppy statements.
(3) Introduction [a.k.a. what others have previously reported; ~1.5-2 pages]. This is not a summary of the laboratory manual introduction. Literature citations (not Websites) in proper format should also be present. Key points of the experiment appear here and often dictate differences A, B, and C grades. This often can be prepared in advance of the laboratory experiment.
(4) Motivation [a.k.a. why other than a grade are you writing this document or why should we care?)]. This is again not a summary of the laboratory manual introduction (~1-2 paragraphs). Include as a portion of the Introduction section. Literature citations (not websites) in proper format should also be present.
(5) Experimental/Physical Methods . This described what purification techniques for reagents, sources, prior literature synthetic details, and instrumentation (model number and any modifications) was used to prepare/characterize your reaction products. (~1-3 paragraphs, abstract style). Literature citations (not websites) in proper format should also be present.
(6) Experimental. Describes the reagent quantities, times, temperatures, and pressures (etc.) used during experiment. Should be accurate and complete so that the experiment may be repeated by another. Yields and additional analysis data must also be present in short format. Use neutral past tense (i.e. no I or we).
(7) Results and Discussion . This section compares your research findings to the primary research literature (i.e. not website or those in lab manual). You should describe what was done, interpret and report your data, and compare your data/conclusions to the primary literature (e.g. published manuscript). Literature citations (not websites) in proper format should also support your claims. (~2-20 pages; judgment call). The length of this section depends on the experimental data and complexity of experiment.
(8) Figures, Tables, and Schemes . These should include experimental data plots (spectra, structures, etc.) or clearly indicate non-trivial chemical transformations in a graphical format. Acid-base neutralization, salt elimination, distillation apparatus, Schlenk line design, etc. are not useful. For examples consult several manuscripts that appear in the Journal of the American Chemical Society.
(9) Conclusions . You should briefly describe why you performed the experiment, what conclusions were drawn, how they agree with or differ from literature reports, and propose a new avenue for study (a.k.a. future directions). This section will be ~ 1-2 paragraphs in length and is not the same as an abstract.
(10) Acknowledgments . You should thank staff, faculty, and students who assisted with data collection, analysis, or experimental issues. Access to facilities outside of the laboratory and their funding sources should also be mentioned.
(11) References. Primary literature citations (minimum = 20) that are used to support claims and assignments contained within the written report. Websites are not allowable sources for citations or information. The references must contain 75% original citations (i.e. other than those described in the laboratory handout or manual). The presence of online citations will result in a grade of zero and the report will be returned. Note: Must use J. Am. Chem. Soc. format. See: http://pubs.acs.org/journal/jacsat
(12) Supporting Information . Includes trivial calculations, Figures, and any additional data that does not appear in the manuscript text.
Report Submission
All students are required to submit their reports (6 total) in PDF (last name_report number.pdf) format as an attached document in a single E-mail to holmesst@umsl.edu . Reports that are deemed too large by E-mail servers (e.g. Hotmail) will require reduction of Figures and/or Schemes data size; submissions via UMSL E-mail servers should not experience this problem. In addition, a complete and legible printed paper copy is to be submitted prior to or on the report due date (Wed. 5:30 PM). If you do not own a copy of Microsoft Word or Adobe Acrobat, this work can be performed within UMSL Chemistry & Biochemistry Computer Lab, 232 Benton Hall). Reports submitted after class are considered as “late” and are subject to a 10% penalty immediately. Each subsequent day (5 PM) is assessed an additional 10% penalty. Reports submitted two or more days (≥ 48 hours) after the due date will not be graded and a grade of “0, zero” will be assigned.
All students are required to submit their reports (6 total) in PDF (last name_report number.pdf) format as an attached document in a single E-mail to holmesst@umsl.edu . Reports that are deemed too large by E-mail servers (e.g. Hotmail) will require reduction of Figures and/or Schemes data size; submissions via UMSL E-mail servers should not experience this problem. In addition, a complete and legible printed paper copy is to be submitted prior to or on the report due date (Wed. 5:30 PM). If you do not own a copy of Microsoft Word or Adobe Acrobat, this work can be performed within UMSL Chemistry & Biochemistry Computer Lab, 232 Benton Hall).
Reports submitted after class are considered as “late” and are subject to a 10% penalty immediately. Each subsequent day (5 PM) is assessed an additional 10% penalty. Reports submitted two or more days (≥ 48 hours) after the due date will not be graded and a grade of “0, zero” will be assigned.
Report Grade Assignment
Report grading will adhere to the following weighting scheme.
Abstract Introduction Results & Discussion Experimental References Notebook Spectra Sample Appearance & Labeling 5 20 20 10 5 10 10 20
Results & Discussion
