data_5132 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H and 15N assignments of ATTm+4, a truncated version of ATT, an trypsin/chymotrypsin inhibitor from Arabidopsis thaliana ; _BMRB_accession_number 5132 _BMRB_flat_file_name bmr5132.str _Entry_type original _Submission_date 2001-09-06 _Accession_date 2001-09-06 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details . loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Zhao Qin . . 2 Chae Young-Kee . . 3 Markley John L. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 207 "15N chemical shifts" 55 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2003-06-10 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 5056 'full-length ATT' 5133 'mature ATT' stop_ _Original_release_date 2001-09-06 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; NMR Solution Structure of ATTp, an Arabidopsis thaliana Trypsin Inhibitor ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code 22257244 _PubMed_ID 12369816 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Zhao Qin . . 2 Chae Young-Kee . . 3 Markley John L. . stop_ _Journal_abbreviation Biochemistry _Journal_volume 41 _Journal_issue 41 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 12284 _Page_last 12296 _Year 2002 _Details . loop_ _Keyword ATT arabidopsis 'trypsin inhibitor' stop_ save_ ################################## # Molecular system description # ################################## save_system_attm+4 _Saveframe_category molecular_system _Mol_system_name attm+4 _Abbreviation_common attm+4 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label attm+4 $attm+4 stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state monomer _System_paramagnetic no _System_thiol_state 'all disulfide bound' loop_ _Biological_function 'trypsin/chymotrypsin inhibitor' stop_ _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_attm+4 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common attm+4 _Abbreviation_common attm+4 _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details ; N-terminal residues: YVEF are cloning artifacts; the sequence is numbered from 3 rather than 1 (for comparison purposes with ATT) ; ############################## # Polymer residue sequence # ############################## _Residue_count 66 _Mol_residue_sequence ; YVEFQGNECLKEYGGDVGFG FCAPRIFPTICYTRCRENKG AKGGRCRWGQGSNVKCLCDF CGDTPQ ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 3 TYR 2 4 VAL 3 5 GLU 4 6 PHE 5 7 GLN 6 8 GLY 7 9 ASN 8 10 GLU 9 11 CYS 10 12 LEU 11 13 LYS 12 14 GLU 13 15 TYR 14 16 GLY 15 17 GLY 16 18 ASP 17 19 VAL 18 20 GLY 19 21 PHE 20 22 GLY 21 23 PHE 22 24 CYS 23 25 ALA 24 26 PRO 25 27 ARG 26 28 ILE 27 29 PHE 28 30 PRO 29 31 THR 30 32 ILE 31 33 CYS 32 34 TYR 33 35 THR 34 36 ARG 35 37 CYS 36 38 ARG 37 39 GLU 38 40 ASN 39 41 LYS 40 42 GLY 41 43 ALA 42 44 LYS 43 45 GLY 44 46 GLY 45 47 ARG 46 48 CYS 47 49 ARG 48 50 TRP 49 51 GLY 50 52 GLN 51 53 GLY 52 54 SER 53 55 ASN 54 56 VAL 55 57 LYS 56 58 CYS 57 59 LEU 58 60 CYS 59 61 ASP 60 62 PHE 61 63 CYS 62 64 GLY 63 65 ASP 64 66 THR 65 67 PRO 66 68 GLN stop_ _Sequence_homology_query_date 2008-08-19 _Sequence_homology_query_revised_last_date 2007-05-31 loop_ _Database_name _Database_accession_code _Database_entry_mol_name _Sequence_query_to_submitted_percentage _Sequence_subject_length _Sequence_identity _Sequence_positive _Sequence_homology_expectation_value BMRB 5133 attm 106.45 62 100 100 2e-34 stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $attm+4 'Thale cress' 3702 Eukaryota Viridiplantae Arabidopsis thaliana 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 $attm+4 'recombinant technology' 'Pichia pastoris' Pichia pastoris GS115 pPIC9k/attp 'Protein secreted to growth media.' 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 $attm+4 1 mM [U-15N] 'sodium acetate' 50 mM [U-2H] DSS 0.1 mM . stop_ save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DMX _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '15N HSQC' _Sample_label . save_ save_15N_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '15N TOCSY' _Sample_label . save_ save_15N_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '15N NOESY' _Sample_label . save_ ####################### # Sample conditions # ####################### save_Ex-cond _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.0 0.2 n/a temperature 298 0.5 K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_ref _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 0.0 internal direct . . . 1.0 DSS N 15 'methyl protons' ppm 0.0 . indirect . . . 0.101329118 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_attm+4 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '15N HSQC' '15N TOCSY' '15N NOESY' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $Ex-cond _Chem_shift_reference_set_label $chemical_shift_ref _Mol_system_component_name attm+4 _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 . 7 ASN HA H 4.634 0.02 . 2 . 7 ASN HB2 H 2.777 0.02 . 3 . 7 ASN HB3 H 2.777 0.02 . 4 . 7 ASN H H 8.32 0.02 . 5 . 7 ASN N N 120.061 0.05 . 6 . 8 GLU HA H 4.234 0.02 . 7 . 8 GLU HB2 H 1.889 0.02 . 8 . 8 GLU HG2 H 2.239 0.02 . 9 . 8 GLU HG3 H 2.239 0.02 . 10 . 8 GLU H H 8.604 0.02 . 11 . 8 GLU N N 121.451 0.05 . 12 . 9 CYS HA H 4.561 0.02 . 13 . 9 CYS HB2 H 3.037 0.02 . 14 . 9 CYS HB3 H 2.937 0.02 . 15 . 9 CYS H H 8.161 0.02 . 16 . 9 CYS N N 118.093 0.05 . 17 . 10 LEU HA H 5.636 0.02 . 18 . 10 LEU HB2 H 1.737 0.02 . 19 . 10 LEU HB3 H 1.143 0.02 . 20 . 10 LEU HD1 H 1.471 0.02 . 21 . 10 LEU HD2 H 0.673 0.02 . 22 . 10 LEU H H 7.784 0.02 . 23 . 10 LEU N N 120.034 0.05 . 24 . 11 LYS HA H 4.669 0.02 . 25 . 11 LYS HB3 H 1.726 0.02 . 26 . 11 LYS H H 8.885 0.02 . 27 . 11 LYS N N 122.77 0.05 . 28 . 12 GLU HA H 4.467 0.02 . 29 . 12 GLU HB2 H 2.018 0.02 . 30 . 12 GLU HG2 H 2.178 0.02 . 31 . 12 GLU H H 9.17 0.02 . 32 . 12 GLU N N 125.797 0.05 . 33 . 13 TYR HA H 3.892 0.02 . 34 . 13 TYR HB2 H 2.851 0.02 . 35 . 13 TYR HB3 H 2.639 0.02 . 36 . 13 TYR H H 8.609 0.02 . 37 . 13 TYR N N 125.501 0.05 . 38 . 14 GLY HA2 H 4.458 0.02 . 39 . 14 GLY HA3 H 3.466 0.02 . 40 . 14 GLY H H 8.466 0.02 . 41 . 14 GLY N N 107.894 0.05 . 42 . 15 GLY HA2 H 4.182 0.02 . 43 . 15 GLY HA3 H 3.757 0.02 . 44 . 15 GLY H H 8.464 0.02 . 45 . 15 GLY N N 113.313 0.05 . 46 . 16 ASP HA H 4.896 0.02 . 47 . 16 ASP HB2 H 2.761 0.02 . 48 . 16 ASP HB3 H 2.456 0.02 . 49 . 16 ASP H H 8.72 0.02 . 50 . 16 ASP N N 123.165 0.05 . 51 . 17 VAL HA H 3.859 0.02 . 52 . 17 VAL HG1 H 0.452 0.02 . 53 . 17 VAL HG2 H 0.119 0.02 . 54 . 17 VAL H H 7.132 0.02 . 55 . 17 VAL N N 112.038 0.05 . 56 . 18 GLY HA2 H 3.675 0.02 . 57 . 18 GLY HA3 H 2.974 0.02 . 58 . 18 GLY H H 8.299 0.02 . 59 . 18 GLY N N 110.158 0.05 . 60 . 19 PHE HA H 3.654 0.02 . 61 . 19 PHE HB3 H 2.929 0.02 . 62 . 19 PHE H H 8.767 0.02 . 63 . 19 PHE N N 123.816 0.05 . 64 . 20 GLY HA2 H 3.818 0.02 . 65 . 20 GLY HA3 H 3.818 0.02 . 66 . 20 GLY H H 8.476 0.02 . 67 . 20 GLY N N 107.014 0.05 . 68 . 21 PHE HA H 4.737 0.02 . 69 . 21 PHE HB2 H 2.93 0.02 . 70 . 21 PHE HB3 H 2.693 0.02 . 71 . 21 PHE H H 7.882 0.02 . 72 . 21 PHE N N 115.872 0.05 . 73 . 22 CYS HA H 4.894 0.02 . 74 . 22 CYS HB2 H 2.828 0.02 . 75 . 22 CYS HB3 H 2.546 0.02 . 76 . 22 CYS H H 8.17 0.02 . 77 . 22 CYS N N 119.08 0.05 . 78 . 23 ALA H H 8.596 0.02 . 79 . 25 ARG HA H 4.271 0.02 . 80 . 25 ARG HD2 H 3.169 0.02 . 81 . 25 ARG HG2 H 1.63 0.02 . 82 . 26 ILE HA H 4.149 0.02 . 83 . 26 ILE HB H 1.553 0.02 . 84 . 26 ILE HG12 H 1.295 0.02 . 85 . 26 ILE H H 7.345 0.02 . 86 . 26 ILE N N 125.081 0.05 . 87 . 27 PHE H H 8.128 0.02 . 88 . 27 PHE N N 125.35 0.05 . 89 . 29 THR HA H 4.149 0.02 . 90 . 29 THR HB H 4.589 0.02 . 91 . 29 THR H H 8.318 0.02 . 92 . 29 THR N N 110.734 0.05 . 93 . 30 ILE HA H 3.472 0.02 . 94 . 30 ILE HB H 2.036 0.02 . 95 . 30 ILE H H 8.248 0.02 . 96 . 30 ILE N N 121.719 0.05 . 97 . 31 CYS HA H 3.882 0.02 . 98 . 31 CYS HB2 H 2.857 0.02 . 99 . 31 CYS HB3 H 2.7 0.02 . 100 . 31 CYS H H 7.139 0.02 . 101 . 31 CYS N N 115.158 0.05 . 102 . 32 TYR HA H 3.384 0.02 . 103 . 32 TYR HB2 H 2.799 0.02 . 104 . 32 TYR H H 7.792 0.02 . 105 . 32 TYR N N 121.775 0.05 . 106 . 33 THR HA H 3.572 0.02 . 107 . 33 THR HB H 3.925 0.02 . 108 . 33 THR H H 7.968 0.02 . 109 . 33 THR N N 117.571 0.05 . 110 . 34 ARG HA H 3.945 0.02 . 111 . 34 ARG HB2 H 1.451 0.02 . 112 . 34 ARG HB3 H 1.205 0.02 . 113 . 34 ARG HD2 H 2.885 0.02 . 114 . 34 ARG HD3 H 2.472 0.02 . 115 . 34 ARG H H 9.179 0.02 . 116 . 34 ARG N N 121.57 0.05 . 117 . 35 CYS HA H 4.126 0.02 . 118 . 35 CYS HB2 H 2.683 0.02 . 119 . 35 CYS HB3 H 2.32 0.02 . 120 . 35 CYS H H 8.569 0.02 . 121 . 35 CYS N N 120.345 0.05 . 122 . 36 ARG HA H 3.896 0.02 . 123 . 36 ARG HB3 H 1.533 0.02 . 124 . 36 ARG H H 7.321 0.02 . 125 . 36 ARG N N 120.908 0.05 . 126 . 37 GLU HA H 3.954 0.02 . 127 . 37 GLU HB2 H 1.898 0.02 . 128 . 37 GLU HB3 H 1.898 0.02 . 129 . 37 GLU HG2 H 2.405 0.02 . 130 . 37 GLU HG3 H 2.162 0.02 . 131 . 37 GLU H H 8.526 0.02 . 132 . 37 GLU N N 117.873 0.05 . 133 . 38 ASN HA H 4.959 0.02 . 134 . 38 ASN HB2 H 3.088 0.02 . 135 . 38 ASN HB3 H 2.893 0.02 . 136 . 38 ASN H H 8.665 0.02 . 137 . 38 ASN N N 113.763 0.05 . 138 . 39 LYS HA H 4.75 0.02 . 139 . 39 LYS HB2 H 2.362 0.02 . 140 . 39 LYS HB3 H 2.098 0.02 . 141 . 39 LYS H H 6.982 0.02 . 142 . 39 LYS N N 115.14 0.05 . 143 . 40 GLY HA2 H 3.92 0.02 . 144 . 40 GLY HA3 H 3.92 0.02 . 145 . 40 GLY H H 7.514 0.02 . 146 . 40 GLY N N 108.736 0.05 . 147 . 41 ALA HA H 3.829 0.02 . 148 . 41 ALA HB H 0.439 0.02 . 149 . 41 ALA H H 7.159 0.02 . 150 . 41 ALA N N 121.206 0.05 . 151 . 42 LYS HA H 4.016 0.02 . 152 . 42 LYS HB2 H 1.414 0.02 . 153 . 42 LYS HB3 H 1.292 0.02 . 154 . 42 LYS H H 7.895 0.02 . 155 . 42 LYS N N 117.663 0.05 . 156 . 43 GLY HA2 H 3.875 0.02 . 157 . 43 GLY HA3 H 2.955 0.02 . 158 . 43 GLY H H 7.323 0.02 . 159 . 43 GLY N N 105.298 0.05 . 160 . 44 GLY HA2 H 4.807 0.02 . 161 . 44 GLY HA3 H 3.844 0.02 . 162 . 44 GLY H H 7.441 0.02 . 163 . 44 GLY N N 110.729 0.05 . 164 . 45 ARG HA H 4.682 0.02 . 165 . 45 ARG HB2 H 1.871 0.02 . 166 . 45 ARG HB3 H 1.871 0.02 . 167 . 45 ARG H H 9.666 0.02 . 168 . 45 ARG N N 121.864 0.05 . 169 . 46 CYS HA H 5.133 0.02 . 170 . 46 CYS HB2 H 3.32 0.02 . 171 . 46 CYS HB3 H 2.2 0.02 . 172 . 46 CYS H H 8.847 0.02 . 173 . 46 CYS N N 123.243 0.05 . 174 . 47 ARG HA H 4.714 0.02 . 175 . 47 ARG HB2 H 1.664 0.02 . 176 . 47 ARG HB3 H 1.664 0.02 . 177 . 47 ARG H H 8.954 0.02 . 178 . 47 ARG N N 127.078 0.05 . 179 . 48 TRP HA H 4.373 0.02 . 180 . 48 TRP HB2 H 3.397 0.02 . 181 . 48 TRP HB3 H 3.096 0.02 . 182 . 48 TRP H H 9.299 0.02 . 183 . 48 TRP N N 133.12 0.05 . 184 . 49 GLY HA2 H 4.426 0.02 . 185 . 49 GLY HA3 H 3.599 0.02 . 186 . 49 GLY H H 8.708 0.02 . 187 . 49 GLY N N 114.208 0.05 . 188 . 50 GLN HA H 4.382 0.02 . 189 . 50 GLN HB2 H 2.074 0.02 . 190 . 50 GLN HB3 H 1.973 0.02 . 191 . 50 GLN H H 8.659 0.02 . 192 . 50 GLN N N 123.941 0.05 . 193 . 51 GLY HA2 H 3.917 0.02 . 194 . 51 GLY HA3 H 3.749 0.02 . 195 . 51 GLY H H 8.842 0.02 . 196 . 51 GLY N N 113.814 0.05 . 197 . 52 SER HA H 4.636 0.02 . 198 . 52 SER HB2 H 3.887 0.02 . 199 . 52 SER HB3 H 3.887 0.02 . 200 . 52 SER H H 8.651 0.02 . 201 . 52 SER N N 120.295 0.05 . 202 . 53 ASN HA H 4.617 0.02 . 203 . 53 ASN HB2 H 2.865 0.02 . 204 . 53 ASN HB3 H 2.756 0.02 . 205 . 53 ASN H H 7.892 0.02 . 206 . 53 ASN N N 121.54 0.05 . 207 . 54 VAL HA H 4.421 0.02 . 208 . 54 VAL HB H 1.072 0.02 . 209 . 54 VAL HG2 H -0.622 0.02 . 210 . 54 VAL H H 7.91 0.02 . 211 . 54 VAL N N 123.357 0.05 . 212 . 55 LYS HA H 4.536 0.02 . 213 . 55 LYS HB2 H 1.478 0.02 . 214 . 55 LYS HB3 H 1.478 0.02 . 215 . 55 LYS H H 7.68 0.02 . 216 . 55 LYS N N 124.471 0.05 . 217 . 56 CYS HA H 4.957 0.02 . 218 . 56 CYS HB2 H 2.728 0.02 . 219 . 56 CYS HB3 H 2.419 0.02 . 220 . 56 CYS H H 9.514 0.02 . 221 . 56 CYS N N 121.587 0.05 . 222 . 57 LEU HA H 4.567 0.02 . 223 . 57 LEU HB2 H 1.829 0.02 . 224 . 57 LEU HB3 H 1.012 0.02 . 225 . 57 LEU H H 9.106 0.02 . 226 . 57 LEU N N 130.213 0.05 . 227 . 58 CYS HA H 5.042 0.02 . 228 . 58 CYS HB2 H 2.926 0.02 . 229 . 58 CYS HB3 H 2.349 0.02 . 230 . 58 CYS H H 8.991 0.02 . 231 . 58 CYS N N 122.275 0.05 . 232 . 59 ASP HA H 5.232 0.02 . 233 . 59 ASP HB2 H 2.438 0.02 . 234 . 59 ASP HB3 H 1.951 0.02 . 235 . 59 ASP H H 7.86 0.02 . 236 . 59 ASP N N 123.159 0.05 . 237 . 60 PHE HA H 4.249 0.02 . 238 . 60 PHE H H 9.706 0.02 . 239 . 60 PHE N N 125.818 0.05 . 240 . 61 CYS HA H 4.499 0.02 . 241 . 61 CYS HB2 H 3.627 0.02 . 242 . 61 CYS HB3 H 3.01 0.02 . 243 . 61 CYS H H 9.197 0.02 . 244 . 61 CYS N N 120.582 0.05 . 245 . 62 GLY HA2 H 3.932 0.02 . 246 . 62 GLY HA3 H 3.825 0.02 . 247 . 62 GLY H H 8.636 0.02 . 248 . 62 GLY N N 111.438 0.05 . 249 . 63 ASP HA H 4.615 0.02 . 250 . 63 ASP HB2 H 2.74 0.02 . 251 . 63 ASP HB3 H 2.472 0.02 . 252 . 63 ASP H H 8.062 0.02 . 253 . 63 ASP N N 119.968 0.05 . 254 . 64 THR HA H 4.448 0.02 . 255 . 64 THR HB H 4.032 0.02 . 256 . 64 THR H H 8.091 0.02 . 257 . 64 THR N N 119.49 0.05 . 258 . 66 GLN HA H 4.146 0.02 . 259 . 66 GLN HB2 H 2.019 0.02 . 260 . 66 GLN HB3 H 1.892 0.02 . 261 . 66 GLN H H 7.457 0.02 . 262 . 66 GLN N N 126.26 0.05 . stop_ save_