data_18999 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; solution structure of allatide O4 in solution ; _BMRB_accession_number 18999 _BMRB_flat_file_name bmr18999.str _Entry_type original _Submission_date 2013-02-03 _Accession_date 2013-02-03 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'conformation 1 of allatide O4 in solution' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 YANG BAI . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 152 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2015-01-12 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 18998 'Allatide O4 Conformation 2' stop_ _Original_release_date 2013-02-07 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Allatides: Smallest Proteinaceous -Amylase Inhibitors from Allamanda oenotheraefolia and Their Expression in Apocynaceae Plants ; _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 BAI YANG . . stop_ _Journal_abbreviation 'J. Biol. Chem.' _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 allatide_conf1 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label allatide_conf1 $allatide_conf1 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_allatide_conf1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common allatide_conf1 _Molecular_mass 3299.954 _Mol_thiol_state . _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 30 _Mol_residue_sequence ; CIAHYGKCDGIINQCCDPWL CTPPIIGFCL ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 CYS 2 2 ILE 3 3 ALA 4 4 HIS 5 5 TYR 6 6 GLY 7 7 LYS 8 8 CYS 9 9 ASP 10 10 GLY 11 11 ILE 12 12 ILE 13 13 ASN 14 14 GLN 15 15 CYS 16 16 CYS 17 17 ASP 18 18 PRO 19 19 TRP 20 20 LEU 21 21 CYS 22 22 THR 23 23 PRO 24 24 PRO 25 25 ILE 26 26 ILE 27 27 GLY 28 28 PHE 29 29 CYS 30 30 LEU 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 $allatide_conf1 Eudicots 52817 Eukaryota Viridiplantae Allamanda oenotheraefolia 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 $allatide_conf1 'purified from the natural source' . Allamanda oenotheraefolia . na 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 _Concentration_min_value _Concentration_max_value _Isotopic_labeling $allatide_conf1 . mM 0.5 1.0 'natural abundance' H2O 90 % . . 'natural abundance' D2O 10 % . . 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CYANA _Saveframe_category software _Name CYANA _Version . loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task refinement 'structure solution' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 700 _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_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 6 . pH pressure 1 . atm temperature 298 . K 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' 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 allatide_conf1 _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 2 2 ILE H H 9.119 0.020 . 2 2 2 ILE HA H 4.161 0.020 . 3 2 2 ILE HB H 1.876 0.020 . 4 2 2 ILE HG12 H 1.368 0.020 . 5 2 2 ILE HG13 H 1.276 0.020 . 6 2 2 ILE HG2 H 1.074 0.020 . 7 2 2 ILE HD1 H 0.821 0.020 . 8 3 3 ALA H H 8.456 0.020 . 9 3 3 ALA HA H 4.996 0.020 . 10 3 3 ALA HB H 1.495 0.020 . 11 4 4 HIS H H 8.397 0.020 . 12 4 4 HIS HA H 3.941 0.020 . 13 4 4 HIS HB2 H 2.797 0.020 . 14 4 4 HIS HB3 H 2.797 0.020 . 15 5 5 TYR H H 7.986 0.020 . 16 5 5 TYR HA H 4.819 0.020 . 17 5 5 TYR HB2 H 3.496 0.020 . 18 5 5 TYR HB3 H 2.345 0.020 . 19 5 5 TYR HE1 H 6.982 0.020 . 20 5 5 TYR HE2 H 7.801 0.020 . 21 6 6 GLY H H 8.644 0.020 . 22 6 6 GLY HA2 H 4.207 0.020 . 23 6 6 GLY HA3 H 3.571 0.020 . 24 7 7 LYS H H 8.343 0.020 . 25 7 7 LYS HA H 4.259 0.020 . 26 7 7 LYS HB2 H 1.725 0.020 . 27 7 7 LYS HG2 H 1.416 0.020 . 28 7 7 LYS HG3 H 1.250 0.020 . 29 7 7 LYS HD2 H 1.572 0.020 . 30 7 7 LYS HD3 H 1.572 0.020 . 31 7 7 LYS HE2 H 2.948 0.020 . 32 7 7 LYS HE3 H 2.736 0.020 . 33 7 7 LYS HZ H 7.477 0.020 . 34 8 8 CYS H H 8.496 0.020 . 35 8 8 CYS HA H 4.849 0.020 . 36 8 8 CYS HB2 H 3.241 0.020 . 37 8 8 CYS HB3 H 2.845 0.020 . 38 9 9 ASP H H 8.434 0.020 . 39 9 9 ASP HA H 5.022 0.020 . 40 9 9 ASP HB2 H 2.811 0.020 . 41 9 9 ASP HB3 H 2.811 0.020 . 42 10 10 GLY H H 8.437 0.020 . 43 10 10 GLY HA2 H 4.288 0.020 . 44 10 10 GLY HA3 H 3.933 0.020 . 45 11 11 ILE H H 8.348 0.020 . 46 11 11 ILE HA H 4.132 0.020 . 47 11 11 ILE HB H 1.865 0.020 . 48 11 11 ILE HG12 H 1.637 0.020 . 49 11 11 ILE HG13 H 1.637 0.020 . 50 11 11 ILE HG2 H 1.148 0.020 . 51 11 11 ILE HD1 H 0.911 0.020 . 52 12 12 ILE H H 8.123 0.020 . 53 12 12 ILE HA H 4.655 0.020 . 54 12 12 ILE HB H 1.872 0.020 . 55 12 12 ILE HG12 H 1.731 0.020 . 56 12 12 ILE HG13 H 1.731 0.020 . 57 12 12 ILE HD1 H 0.872 0.020 . 58 13 13 ASN H H 9.607 0.020 . 59 13 13 ASN HA H 3.714 0.020 . 60 13 13 ASN HB2 H 3.293 0.020 . 61 13 13 ASN HB3 H 3.048 0.020 . 62 13 13 ASN HD21 H 6.262 0.020 . 63 13 13 ASN HD22 H 6.619 0.020 . 64 14 14 GLN H H 8.644 0.020 . 65 14 14 GLN HA H 4.534 0.020 . 66 14 14 GLN HB2 H 2.146 0.020 . 67 14 14 GLN HB3 H 1.907 0.020 . 68 14 14 GLN HG2 H 2.862 0.020 . 69 14 14 GLN HG3 H 2.314 0.020 . 70 14 14 GLN HE21 H 6.947 0.020 . 71 14 14 GLN HE22 H 8.081 0.020 . 72 15 15 CYS H H 8.744 0.020 . 73 15 15 CYS HA H 4.877 0.020 . 74 15 15 CYS HB2 H 2.768 0.020 . 75 15 15 CYS HB3 H 2.667 0.020 . 76 16 16 CYS H H 10.077 0.020 . 77 16 16 CYS HA H 4.621 0.020 . 78 16 16 CYS HB2 H 3.424 0.020 . 79 16 16 CYS HB3 H 2.616 0.020 . 80 17 17 ASP H H 8.683 0.020 . 81 17 17 ASP HA H 5.534 0.020 . 82 17 17 ASP HB2 H 2.746 0.020 . 83 17 17 ASP HB3 H 2.563 0.020 . 84 19 19 TRP H H 8.781 0.020 . 85 19 19 TRP HA H 4.740 0.020 . 86 19 19 TRP HB2 H 2.325 0.020 . 87 19 19 TRP HB3 H 1.875 0.020 . 88 19 19 TRP HD1 H 6.929 0.020 . 89 19 19 TRP HE1 H 9.721 0.020 . 90 20 20 LEU H H 8.713 0.020 . 91 20 20 LEU HA H 4.557 0.020 . 92 20 20 LEU HB2 H 1.824 0.020 . 93 20 20 LEU HB3 H 1.824 0.020 . 94 20 20 LEU HG H 1.626 0.020 . 95 20 20 LEU HD1 H 1.034 0.020 . 96 20 20 LEU HD2 H 1.034 0.020 . 97 21 21 CYS H H 8.047 0.020 . 98 21 21 CYS HA H 4.097 0.020 . 99 21 21 CYS HB2 H 3.203 0.020 . 100 21 21 CYS HB3 H 2.989 0.020 . 101 22 22 THR H H 9.382 0.020 . 102 22 22 THR HA H 4.434 0.020 . 103 22 22 THR HB H 4.308 0.020 . 104 22 22 THR HG2 H 1.264 0.020 . 105 23 23 PRO HA H 5.142 0.020 . 106 23 23 PRO HB2 H 2.243 0.020 . 107 23 23 PRO HB3 H 2.587 0.020 . 108 23 23 PRO HG2 H 2.021 0.020 . 109 23 23 PRO HG3 H 2.021 0.020 . 110 23 23 PRO HD2 H 3.970 0.020 . 111 23 23 PRO HD3 H 3.662 0.020 . 112 24 24 PRO HA H 3.976 0.020 . 113 24 24 PRO HB2 H 2.035 0.020 . 114 24 24 PRO HB3 H 2.331 0.020 . 115 24 24 PRO HG2 H 1.817 0.020 . 116 24 24 PRO HG3 H 1.817 0.020 . 117 24 24 PRO HD2 H 3.849 0.020 . 118 24 24 PRO HD3 H 3.585 0.020 . 119 25 25 ILE H H 7.997 0.020 . 120 25 25 ILE HA H 5.364 0.020 . 121 25 25 ILE HB H 1.814 0.020 . 122 25 25 ILE HG12 H 1.436 0.020 . 123 25 25 ILE HG13 H 1.436 0.020 . 124 25 25 ILE HG2 H 1.065 0.020 . 125 25 25 ILE HD1 H 0.894 0.020 . 126 26 26 ILE H H 7.824 0.020 . 127 26 26 ILE HA H 4.389 0.020 . 128 26 26 ILE HB H 1.908 0.020 . 129 26 26 ILE HG12 H 1.397 0.020 . 130 26 26 ILE HG13 H 1.397 0.020 . 131 26 26 ILE HG2 H 1.046 0.020 . 132 26 26 ILE HD1 H 0.862 0.020 . 133 27 27 GLY H H 7.701 0.020 . 134 27 27 GLY HA2 H 4.100 0.020 . 135 27 27 GLY HA3 H 4.100 0.020 . 136 28 28 PHE H H 8.221 0.020 . 137 28 28 PHE HA H 5.485 0.020 . 138 28 28 PHE HB2 H 2.746 0.020 . 139 28 28 PHE HB3 H 2.610 0.020 . 140 28 28 PHE HD1 H 7.304 0.020 . 141 28 28 PHE HD2 H 7.304 0.020 . 142 28 28 PHE HZ H 7.373 0.020 . 143 29 29 CYS H H 8.885 0.020 . 144 29 29 CYS HA H 4.845 0.020 . 145 29 29 CYS HB2 H 2.974 0.020 . 146 29 29 CYS HB3 H 2.763 0.020 . 147 30 30 LEU H H 9.421 0.020 . 148 30 30 LEU HA H 4.683 0.020 . 149 30 30 LEU HB2 H 1.583 0.020 . 150 30 30 LEU HB3 H 1.583 0.020 . 151 30 30 LEU HG H 1.458 0.020 . 152 30 30 LEU HD1 H 0.887 0.020 . stop_ save_