data_30750 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR solution structure of leech peptide HSTX-I ; _BMRB_accession_number 30750 _BMRB_flat_file_name bmr30750.str _Entry_type original _Submission_date 2020-04-29 _Accession_date 2020-04-29 _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 Schroeder C. I. . 2 McMahon K. L. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 131 "13C chemical shifts" 62 "15N chemical shifts" 16 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2020-06-19 original BMRB . stop_ _Original_release_date 2020-05-26 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; Pharmacological activity and NMR solution structure of the leech peptide HSTX-I ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 32524995 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 McMahon Kirsten L. . 2 Tay Bryan . . 3 Deuis Jennifer R. . 4 Tanaka Brian S. . 5 Peigneur Steve . . 6 Jin Ai-Hua H. . 7 Tytgat Jan . . 8 Waxman Stephen G. . 9 Dib-Hajj Sulayman D. . 10 Vetter Irina . . 11 Schroeder Christina I. . stop_ _Journal_abbreviation 'Biochem. Pharmacol.' _Journal_name_full 'Biochemical pharmacology' _Journal_volume . _Journal_issue . _Journal_ISSN 1873-2968 _Journal_CSD 0353 _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 114082 _Page_last 114082 _Year 2020 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name HSTX-I _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label unit_1 $entity_1 stop_ _System_molecular_weight . _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_entity_1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1 _Molecular_mass 2625.178 _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 24 _Mol_residue_sequence ; ACKEYWECGAFLFCIEGICV PMIX ; loop_ _Residue_seq_code _Residue_label 1 ALA 2 CYS 3 LYS 4 GLU 5 TYR 6 TRP 7 GLU 8 CYS 9 GLY 10 ALA 11 PHE 12 LEU 13 PHE 14 CYS 15 ILE 16 GLU 17 GLY 18 ILE 19 CYS 20 VAL 21 PRO 22 MET 23 ILE 24 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_NH2 _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common 'AMINO GROUP' _BMRB_code NH2 _PDB_code NH2 _Standard_residue_derivative . _Molecular_mass 16.023 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? HN1 HN1 H . 0 . ? HN2 HN2 H . 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name SING N HN1 ? ? SING N HN2 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $entity_1 'Indian leech' 13555 Eukaryota Metazoa Haemadipsa sylvestris 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_1 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '2 mg/mL HSTX-I, 67% H2O/33% ACN-d3' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 2 mg/mL 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details '2 mg/mL HSTX-I, 67% D2O/33% ACN-d3' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 2 mg/mL 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name TopSpin _Version . loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection processing stop_ _Details . save_ save_software_2 _Saveframe_category software _Name 'CcpNmr Analysis' _Version . loop_ _Vendor _Address _Electronic_address CCPN . . stop_ loop_ _Task 'chemical shift assignment' 'peak picking' stop_ _Details . save_ save_software_3 _Saveframe_category software _Name CYANA _Version . loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task 'structure calculation' stop_ _Details . save_ save_software_4 _Saveframe_category software _Name CNS _Version . 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_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model 'AVANCE III' _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_1D_1 _Saveframe_category NMR_applied_experiment _Experiment_name 1D _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_1D_5 _Saveframe_category NMR_applied_experiment _Experiment_name 1D _Sample_label $sample_2 save_ save_2D_1H-13C_HSQC_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_2 save_ save_2D_1H-1H_NOESY_7 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_2 save_ save_2D_1H-1H_TOCSY_8 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_2 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 4 . pH pressure 1 . atm temperature 298 . K stop_ save_ save_sample_conditions_2 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 4 . pH pressure 1 . atm temperature 298 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_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 water H 1 protons ppm 4.76 internal direct . . . 1.0 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_chemical_shifts_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label 1D '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '2D 1H-15N HSQC' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name unit_1 _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 ALA HA H 3.990 0.003 . 2 1 1 ALA HB H 1.418 0.002 . 3 1 1 ALA CA C 52.248 0.000 . 4 1 1 ALA CB C 19.862 0.000 . 5 2 2 CYS HA H 4.508 0.003 . 6 2 2 CYS HB2 H 3.176 0.002 . 7 2 2 CYS HB3 H 2.916 0.003 . 8 2 2 CYS CA C 56.333 0.000 . 9 2 2 CYS CB C 43.447 0.025 . 10 3 3 LYS H H 8.442 0.003 . 11 3 3 LYS HA H 4.140 0.004 . 12 3 3 LYS HB2 H 1.713 0.003 . 13 3 3 LYS HB3 H 1.713 0.003 . 14 3 3 LYS HG2 H 1.326 0.001 . 15 3 3 LYS HG3 H 1.326 0.001 . 16 3 3 LYS HD2 H 1.590 0.001 . 17 3 3 LYS HD3 H 1.590 0.001 . 18 3 3 LYS HE2 H 2.903 0.002 . 19 3 3 LYS HE3 H 2.903 0.002 . 20 3 3 LYS CA C 57.290 0.000 . 21 3 3 LYS CB C 33.929 0.000 . 22 3 3 LYS CG C 25.420 0.000 . 23 3 3 LYS CD C 29.492 0.000 . 24 3 3 LYS CE C 42.405 0.000 . 25 3 3 LYS N N 122.837 0.000 . 26 4 4 GLU H H 7.579 0.001 . 27 4 4 GLU HA H 4.250 0.004 . 28 4 4 GLU HB2 H 1.351 0.008 . 29 4 4 GLU HB3 H 1.247 0.008 . 30 4 4 GLU HG2 H 2.077 0.004 . 31 4 4 GLU HG3 H 2.077 0.004 . 32 4 4 GLU CA C 55.339 0.000 . 33 4 4 GLU CB C 30.511 0.013 . 34 4 4 GLU CG C 35.276 0.000 . 35 4 4 GLU N N 116.571 0.000 . 36 5 5 TYR H H 8.160 0.003 . 37 5 5 TYR HA H 4.064 0.001 . 38 5 5 TYR HB2 H 2.940 0.003 . 39 5 5 TYR HB3 H 2.841 0.003 . 40 5 5 TYR HD1 H 6.885 0.002 . 41 5 5 TYR HD2 H 6.885 0.002 . 42 5 5 TYR HE1 H 6.693 0.000 . 43 5 5 TYR HE2 H 6.693 0.000 . 44 5 5 TYR CA C 61.380 0.000 . 45 5 5 TYR CB C 38.654 0.002 . 46 5 5 TYR N N 120.863 0.000 . 47 6 6 TRP H H 7.236 0.001 . 48 6 6 TRP HA H 4.373 0.004 . 49 6 6 TRP HB2 H 3.296 0.005 . 50 6 6 TRP HB3 H 3.075 0.005 . 51 6 6 TRP HD1 H 7.129 0.002 . 52 6 6 TRP HE1 H 10.157 0.007 . 53 6 6 TRP HE3 H 7.197 0.003 . 54 6 6 TRP HZ2 H 7.386 0.004 . 55 6 6 TRP HZ3 H 7.018 0.001 . 56 6 6 TRP HH2 H 7.131 0.004 . 57 6 6 TRP CA C 58.769 0.000 . 58 6 6 TRP CB C 28.910 0.008 . 59 6 6 TRP N N 116.495 0.000 . 60 6 6 TRP NE1 N 130.088 0.000 . 61 7 7 GLU H H 7.371 0.003 . 62 7 7 GLU HA H 4.130 0.002 . 63 7 7 GLU HB2 H 1.928 0.007 . 64 7 7 GLU HB3 H 1.785 0.019 . 65 7 7 GLU HG2 H 1.931 0.011 . 66 7 7 GLU CA C 58.201 0.000 . 67 7 7 GLU CB C 30.285 0.004 . 68 7 7 GLU CG C 35.299 0.037 . 69 7 7 GLU N N 118.096 0.000 . 70 8 8 CYS H H 7.664 0.001 . 71 8 8 CYS HA H 4.624 0.003 . 72 8 8 CYS HB2 H 3.172 0.004 . 73 8 8 CYS HB3 H 3.057 0.002 . 74 8 8 CYS CA C 56.478 0.000 . 75 8 8 CYS CB C 42.793 0.008 . 76 8 8 CYS N N 115.528 0.000 . 77 9 9 GLY H H 7.914 0.002 . 78 9 9 GLY HA2 H 3.737 0.003 . 79 9 9 GLY HA3 H 3.855 0.002 . 80 9 9 GLY CA C 45.964 0.002 . 81 9 9 GLY N N 108.149 0.000 . 82 10 10 ALA H H 7.730 0.003 . 83 10 10 ALA HA H 4.506 0.010 . 84 10 10 ALA HB H 1.167 0.002 . 85 10 10 ALA CA C 52.404 0.000 . 86 10 10 ALA CB C 21.060 0.000 . 87 11 11 PHE H H 8.234 0.002 . 88 11 11 PHE HA H 4.852 0.001 . 89 11 11 PHE HB2 H 3.104 0.002 . 90 11 11 PHE HB3 H 2.974 0.001 . 91 11 11 PHE CB C 41.248 0.010 . 92 12 12 LEU HA H 4.699 0.010 . 93 12 12 LEU HB2 H 1.515 0.006 . 94 12 12 LEU HB3 H 1.319 0.004 . 95 12 12 LEU HG H 0.738 0.002 . 96 12 12 LEU HD1 H 0.653 0.000 . 97 12 12 LEU HD2 H 0.652 0.000 . 98 12 12 LEU CB C 45.388 0.058 . 99 12 12 LEU CG C 25.829 0.000 . 100 12 12 LEU CD1 C 24.415 0.000 . 101 12 12 LEU CD2 C 24.415 0.000 . 102 13 13 PHE H H 8.754 0.001 . 103 13 13 PHE HA H 4.890 0.015 . 104 13 13 PHE HB2 H 2.974 0.004 . 105 13 13 PHE HB3 H 2.974 0.004 . 106 13 13 PHE HD1 H 7.230 0.002 . 107 13 13 PHE HD2 H 7.230 0.002 . 108 13 13 PHE HE1 H 7.155 0.000 . 109 13 13 PHE HE2 H 7.155 0.000 . 110 13 13 PHE CA C 57.086 0.000 . 111 13 13 PHE CB C 41.822 0.000 . 112 14 14 CYS H H 8.150 0.003 . 113 14 14 CYS HA H 5.528 0.002 . 114 14 14 CYS HB2 H 2.835 0.001 . 115 14 14 CYS HB3 H 2.528 0.001 . 116 14 14 CYS CB C 49.188 0.019 . 117 15 15 ILE H H 8.510 0.005 . 118 15 15 ILE HA H 4.054 0.003 . 119 15 15 ILE HB H 1.583 0.002 . 120 15 15 ILE HG12 H 1.307 0.002 . 121 15 15 ILE HG13 H 1.307 0.002 . 122 15 15 ILE HG2 H 0.820 0.003 . 123 15 15 ILE HD1 H 0.868 0.002 . 124 15 15 ILE CA C 61.003 0.000 . 125 15 15 ILE CB C 41.463 0.000 . 126 15 15 ILE CG1 C 28.522 0.000 . 127 15 15 ILE CD1 C 14.240 0.000 . 128 15 15 ILE N N 121.356 0.000 . 129 16 16 GLU H H 8.861 0.003 . 130 16 16 GLU HA H 3.678 0.007 . 131 16 16 GLU HB2 H 2.244 0.005 . 132 16 16 GLU HB3 H 1.923 0.006 . 133 16 16 GLU HG2 H 2.328 0.013 . 134 16 16 GLU HG3 H 2.311 0.011 . 135 16 16 GLU CA C 57.331 0.000 . 136 16 16 GLU CB C 27.632 0.003 . 137 16 16 GLU CG C 34.799 0.001 . 138 16 16 GLU N N 123.065 0.000 . 139 17 17 GLY H H 8.008 0.003 . 140 17 17 GLY HA2 H 3.438 0.017 . 141 17 17 GLY HA3 H 4.001 0.016 . 142 17 17 GLY CA C 45.850 0.008 . 143 17 17 GLY N N 103.084 0.000 . 144 18 18 ILE H H 7.839 0.004 . 145 18 18 ILE HA H 4.260 0.002 . 146 18 18 ILE HB H 1.979 0.003 . 147 18 18 ILE HG12 H 1.451 0.001 . 148 18 18 ILE HG13 H 1.122 0.001 . 149 18 18 ILE HG2 H 0.809 0.000 . 150 18 18 ILE HD1 H 0.809 0.002 . 151 18 18 ILE CA C 60.508 0.000 . 152 18 18 ILE CB C 39.284 0.000 . 153 18 18 ILE CG1 C 27.595 0.009 . 154 18 18 ILE CD1 C 13.758 0.000 . 155 18 18 ILE N N 121.431 0.000 . 156 19 19 CYS H H 8.267 0.004 . 157 19 19 CYS HA H 5.556 0.005 . 158 19 19 CYS HB2 H 2.849 0.002 . 159 19 19 CYS HB3 H 2.558 0.007 . 160 19 19 CYS CA C 55.403 0.000 . 161 19 19 CYS CB C 48.241 0.004 . 162 19 19 CYS N N 123.468 0.000 . 163 20 20 VAL H H 8.884 0.005 . 164 20 20 VAL HA H 4.743 0.003 . 165 20 20 VAL HB H 2.165 0.003 . 166 20 20 VAL HG1 H 0.973 0.004 . 167 20 20 VAL HG2 H 0.975 0.005 . 168 20 20 VAL CA C 58.585 0.000 . 169 20 20 VAL CB C 35.091 0.000 . 170 20 20 VAL CG1 C 22.098 0.000 . 171 20 20 VAL CG2 C 20.282 0.000 . 172 21 21 PRO HA H 4.720 0.009 . 173 21 21 PRO HB2 H 2.083 0.004 . 174 21 21 PRO HB3 H 1.846 0.002 . 175 21 21 PRO HG2 H 2.081 0.003 . 176 21 21 PRO HG3 H 1.845 0.002 . 177 21 21 PRO HD2 H 3.692 0.001 . 178 21 21 PRO HD3 H 3.692 0.001 . 179 21 21 PRO CA C 63.215 0.000 . 180 21 21 PRO CB C 32.686 0.016 . 181 21 21 PRO CG C 28.131 0.004 . 182 21 21 PRO CD C 51.417 0.000 . 183 22 22 MET H H 8.425 0.005 . 184 22 22 MET HA H 4.482 0.011 . 185 22 22 MET HB2 H 1.824 0.002 . 186 22 22 MET HB3 H 1.631 0.007 . 187 22 22 MET HG2 H 2.368 0.012 . 188 22 22 MET HG3 H 2.368 0.012 . 189 22 22 MET HE H 1.890 0.000 . 190 22 22 MET CA C 55.472 0.000 . 191 22 22 MET CB C 35.015 0.000 . 192 22 22 MET CG C 33.088 0.000 . 193 22 22 MET CE C 17.820 0.000 . 194 22 22 MET N N 120.764 0.000 . 195 23 23 ILE H H 7.673 0.002 . 196 23 23 ILE HA H 4.210 0.005 . 197 23 23 ILE HB H 1.762 0.002 . 198 23 23 ILE HG12 H 1.414 0.001 . 199 23 23 ILE HG13 H 1.099 0.009 . 200 23 23 ILE HG2 H 0.863 0.003 . 201 23 23 ILE HD1 H 0.812 0.002 . 202 23 23 ILE CA C 60.865 0.000 . 203 23 23 ILE CB C 39.724 0.000 . 204 23 23 ILE CG1 C 27.866 0.000 . 205 23 23 ILE CG2 C 18.266 0.000 . 206 23 23 ILE N N 119.812 0.000 . 207 24 24 NH2 N N 109.688 0.000 . 208 24 24 NH2 HN1 H 7.465 0.000 . 209 24 24 NH2 HN2 H 6.815 0.000 . stop_ save_