data_5934 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 13C and 15N Chemical Shift Assignments for f-MLF-OH ; _BMRB_accession_number 5934 _BMRB_flat_file_name bmr5934.str _Entry_type original _Submission_date 2003-09-05 _Accession_date 2003-09-05 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'Chemical shifts obtained on microcrystalline sample at room temperature' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Rienstra Chad M. . 2 Griffin Robert G. . 3 Lozano-Perez Thomas . . 4 Tidor Bruce . . 5 McMahon Michael T. . 6 Reif Bernd . . 7 Hohwy Morten . . 8 Tucker-Kellogg Lisa . . 9 Jaroniec Chris P. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "13C chemical shifts" 17 "15N chemical shifts" 3 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2003-10-16 original author . stop_ _Original_release_date 2003-10-16 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; De novo determination of peptide structure with solid-state magic-angle spinning NMR spectroscopy ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 12149447 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Rienstra Chad M. . 2 Griffin Robert G. . 3 Lozano-Perez Thomas . . 4 Tidor Bruce . . 5 McMahon Michael T. . 6 Reif Bernd . . 7 Hohwy Morten . . 8 Tucker-Kellogg Lisa . . 9 Jaroniec Chris P. . stop_ _Journal_abbreviation 'Proc. Natl. Acad. Sci. U. S. A.' _Journal_volume 99 _Journal_issue . _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 10260 _Page_last 10265 _Year 2002 _Details . loop_ _Keyword f-MLF-OH 'peptide structure with NMR' stop_ save_ ################################## # Molecular system description # ################################## save_MLF _Saveframe_category molecular_system _Mol_system_name 'f-MLF peptide' _Abbreviation_common MLF _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label f-MLF $f-MLF stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state monomer _System_paramagnetic no _System_thiol_state 'not present' _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_f-MLF _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common 'formyl Methionine-Leucine-Phenylalanine' _Abbreviation_common f-MLF _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 3 _Mol_residue_sequence MLF loop_ _Residue_seq_code _Residue_label 1 MET 2 LEU 3 PHE stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $f-MLF . . Eubacteria . . . stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name _Details $f-MLF 'chemical synthesis' . . . . . 'synthesized by standard solid-phase methods and HPLC purification' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solid _Details 'microcrystals grown by overnight evaporation from 2-Propanol' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $f-MLF . mM . stop_ save_ ############################ # Computer software used # ############################ save_RNMR _Saveframe_category software _Name RNMR _Version . loop_ _Task 'spectral processing' assignments stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer 'Cambridge Instruments spectrometers' _Model . _Field_strength 500 _Details . save_ save_NMR_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer 'Cambridge Instruments spectrometers' _Model . _Field_strength 400 _Details . save_ ############################# # NMR applied experiments # ############################# save_C-C_carried_out_using_SPC5,_SPC53_recoupling_1 _Saveframe_category NMR_applied_experiment _Experiment_name 'C-C carried out using SPC5, SPC53 recoupling' _Sample_label $sample_1 save_ save_N-C_experiments_carried_out_using_Specific_CP_2 _Saveframe_category NMR_applied_experiment _Experiment_name 'N-C experiments carried out using Specific CP' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_condition_1 _Saveframe_category sample_conditions _Details 'spin rate ~9kHz' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH . . n/a temperature 305 5 K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference _Saveframe_category chemical_shift_reference _Details . loop_ _Mol_common_name _Atom_type _Atom_isotope_number _Atom_group _Chem_shift_units _Chem_shift_value _Reference_method _Reference_type _External_reference_sample_geometry _External_reference_location _External_reference_axis _Indirect_shift_ratio DSS N 15 'methyl protons' ppm 0.0 . indirect . . . 0.101329118 DSS C 13 'methyl protons' ppm 0.0 . indirect . . . 0.251449530 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_shift_set_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $condition_1 _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name f-MLF _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 . 1 MET C C 172.2 0.1 1 2 . 1 MET CA C 52.0 0.1 1 3 . 1 MET CB C 37.9 0.1 1 4 . 1 MET CG C 28.6 0.1 1 5 . 1 MET CE C 14.0 0.1 1 6 . 1 MET N N 125.5 0.1 1 7 . 2 LEU C C 175.2 0.1 1 8 . 2 LEU CA C 56.8 0.1 1 9 . 2 LEU CB C 40.7 0.1 1 10 . 2 LEU CG C 25.6 0.1 1 11 . 2 LEU CD1 C 24.9 0.1 4 12 . 2 LEU CD2 C 19.6 0.1 4 13 . 2 LEU N N 116.2 0.1 1 14 . 3 PHE C C 173.5 0.1 1 15 . 3 PHE CA C 54.4 0.1 1 16 . 3 PHE CB C 36.9 0.1 1 17 . 3 PHE CG C 136.2 0.1 1 18 . 3 PHE CD1 C 128.1 0.1 1 19 . 3 PHE CD2 C 128.1 0.1 1 20 . 3 PHE N N 107.6 0.1 1 stop_ loop_ _Atom_shift_assign_ID_ambiguity 12 11 stop_ save_