data_21056 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; SFTI-TCTR N12 N14 NMeSer6 ; _BMRB_accession_number 21056 _BMRB_flat_file_name bmr21056.str _Entry_type new _Submission_date 2014-10-21 _Accession_date 2014-11-28 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'Sunflower Trypsin Inhibitor with substitutions: R2T, K5R, F12N, D14N and NMeSer6' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 'de Veer' Simon J. . 2 Swedberg Joakim E. . 3 Akcan Muharrem . . 4 Rosengren Johan K. . 5 Brattsand Maria . . 6 Craik David J. . 7 Harris Jonathan M. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 79 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2015-03-27 original author . stop_ loop_ _Related_BMRB_accession_number _Relationship 21057 'SFTI-TCTR N12 N14' stop_ _Original_release_date 2015-03-27 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Putting Proteases into Reverse Gear: the Role of Sequence and Conformation in Laskowski Mechanism Inhibition' _Citation_status 'in preparation' _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID ? loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 'de Veer' Simon J . 2 Swedberg Joakim E . 3 Akcan Muharrem . . 4 Rosengren Johan K . 5 Brattsand Maria . . 6 Craik David J . 7 Harris Jonathan M . stop_ _Journal_abbreviation 'Not known' _Journal_volume . _Journal_issue . _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first . _Page_last . _Year . _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'SFTI-TCTR N12 N14 NMeSer6' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'SFTI-TCTR N12 N14 NMeSer6' $entity stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_entity _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity _Molecular_mass 1564.715 _Mol_thiol_state 'all disulfide bound' loop_ _Biological_function 'Serine Protease Inhibitor' stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 14 _Mol_residue_sequence GTCTRXIPPICNPN loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 GLY 2 2 THR 3 3 CYS 4 4 THR 5 5 ARG 6 6 MLS 7 7 ILE 8 8 PRO 9 9 PRO 10 10 ILE 11 11 CYS 12 12 ASN 13 13 PRO 14 14 ASN stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_MLS _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common N-METHYL-L-SERINE _BMRB_code MLS _PDB_code MLS _Standard_residue_derivative . _Molecular_mass 119.119 _Mol_paramagnetic . _Details 'We can not find any standard abbreviation for N-methylated Ser. For N-methylated His its MHS so we named it MSR.' save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $entity . . . . . . 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 $entity 'recombinant technology' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity 3 mg 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CYANA _Saveframe_category software _Name CYANA _Version 3.0 loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version 2.1 loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection processing stop_ _Details . save_ save_CCPNMR _Saveframe_category software _Name CCPNMR _Version . loop_ _Vendor _Address _Electronic_address CCPN . . stop_ loop_ _Task 'peak picking' 'chemical shift assignment' stop_ _Details . save_ save_CNS _Saveframe_category software _Name CNS _Version 1.2 loop_ _Vendor _Address _Electronic_address 'Brunger, Adams, Clore, Gros, Nilges and Read' . . stop_ loop_ _Task refinement stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_TOCSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_DQF-COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 298 . K pH 3.7 . pH stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference_1 _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 H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 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_assigned_chem_shift_list_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '2D DQF-COSY' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'SFTI-TCTR N12 N14 NMeSer6' _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 1 GLY H H 7.83 0.01 . 2 1 1 GLY HA2 H 3.77 0.01 . 3 1 1 GLY HA3 H 3.77 0.01 . 4 2 2 THR H H 7.46 0.01 . 5 2 2 THR HA H 4.54 0.01 . 6 2 2 THR HB H 4.00 0.01 . 7 2 2 THR HG2 H 1.08 0.01 . 8 3 3 CYS H H 8.68 0.01 . 9 3 3 CYS HA H 5.47 0.01 . 10 3 3 CYS HB2 H 2.88 0.01 . 11 3 3 CYS HB3 H 2.62 0.01 . 12 4 4 THR H H 8.78 0.01 . 13 4 4 THR HA H 4.44 0.01 . 14 4 4 THR HB H 3.88 0.01 . 15 4 4 THR HG2 H 1.19 0.01 . 16 5 5 ARG H H 8.63 0.01 . 17 5 5 ARG HA H 4.17 0.01 . 18 5 5 ARG HB2 H 1.96 0.01 . 19 5 5 ARG HB3 H 1.76 0.01 . 20 5 5 ARG HD2 H 3.12 0.01 . 21 5 5 ARG HD3 H 3.12 0.01 . 22 5 5 ARG HE H 7.61 0.01 . 23 5 5 ARG HG2 H 1.55 0.01 . 24 5 5 ARG HG3 H 1.55 0.01 . 25 6 6 MLS HN1 H 2.54 0.01 . 26 6 6 MLS HN2 H 2.54 0.01 . 27 6 6 MLS HN3 H 2.54 0.01 . 28 6 6 MLS HA H 4.59 0.01 . 29 6 6 MLS HB2 H 4.19 0.01 . 30 6 6 MLS HB3 H 4.05 0.01 . 31 7 7 ILE H H 8.87 0.01 . 32 7 7 ILE HA H 4.42 0.01 . 33 7 7 ILE HB H 1.82 0.01 . 34 7 7 ILE HD1 H 0.89 0.01 . 35 7 7 ILE HG12 H 1.50 0.01 . 36 7 7 ILE HG13 H 1.50 0.01 . 37 7 7 ILE HG2 H 1.10 0.01 . 38 8 8 PRO HA H 4.96 0.01 . 39 8 8 PRO HB2 H 2.23 0.01 . 40 8 8 PRO HB3 H 2.16 0.01 . 41 8 8 PRO HD2 H 3.38 0.01 . 42 8 8 PRO HD3 H 3.51 0.01 . 43 8 8 PRO HG2 H 1.81 0.01 . 44 8 8 PRO HG3 H 1.81 0.01 . 45 9 9 PRO HA H 4.47 0.01 . 46 9 9 PRO HB2 H 1.98 0.01 . 47 9 9 PRO HB3 H 1.98 0.01 . 48 9 9 PRO HD2 H 3.60 0.01 . 49 9 9 PRO HD3 H 3.60 0.01 . 50 9 9 PRO HG2 H 1.71 0.01 . 51 9 9 PRO HG3 H 1.71 0.01 . 52 10 10 ILE H H 7.69 0.01 . 53 10 10 ILE HA H 4.46 0.01 . 54 10 10 ILE HB H 1.62 0.01 . 55 10 10 ILE HD1 H 0.79 0.01 . 56 10 10 ILE HG2 H 1.09 0.01 . 57 11 11 CYS H H 8.89 0.01 . 58 11 11 CYS HA H 5.32 0.01 . 59 11 11 CYS HB2 H 2.75 0.01 . 60 11 11 CYS HB3 H 2.75 0.01 . 61 12 12 ASN H H 8.55 0.01 . 62 12 12 ASN HA H 4.94 0.01 . 63 12 12 ASN HB2 H 2.72 0.01 . 64 12 12 ASN HB3 H 2.72 0.01 . 65 12 12 ASN HD21 H 7.51 0.01 . 66 12 12 ASN HD22 H 7.22 0.01 . 67 13 13 PRO HA H 4.21 0.01 . 68 13 13 PRO HB2 H 2.22 0.01 . 69 13 13 PRO HB3 H 1.79 0.01 . 70 13 13 PRO HD2 H 3.70 0.01 . 71 13 13 PRO HD3 H 3.70 0.01 . 72 13 13 PRO HG2 H 2.00 0.01 . 73 13 13 PRO HG3 H 1.92 0.01 . 74 14 14 ASN H H 8.06 0.01 . 75 14 14 ASN HA H 4.37 0.01 . 76 14 14 ASN HB2 H 2.72 0.01 . 77 14 14 ASN HB3 H 2.65 0.01 . 78 14 14 ASN HD21 H 7.51 0.01 . 79 14 14 ASN HD22 H 7.01 0.01 . stop_ save_