data_50161 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Backbone 1H, 13C, and 15N Chemical Shift Assignments for hyen D ; _BMRB_accession_number 50161 _BMRB_flat_file_name bmr50161.str _Entry_type original _Submission_date 2020-01-21 _Accession_date 2020-01-21 _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 Du Qingdan . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 165 "13C chemical shifts" 80 "15N chemical shifts" 25 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2020-09-03 update BMRB 'update entry citation' 2020-05-13 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 50162 'hyen L' 50163 'hyen E' 50164 'hyen M' 50165 'hyen C' stop_ _Original_release_date 2020-02-06 save_ ############################# # Citation for this entry # ############################# save_citations_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; Discovery and mechanistic studies of cytotoxic cyclotides from the medicinal herb Hybanthus enneaspermus ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 32414842 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Du Qingdan . . 2 Chan Lai Y. . 3 Gilding Edward K. . 4 Henriques 'Sonia Troeira' T. . 5 Condon Nicholas D. . 6 Ravipati Anjaneya S. . 7 Kaas Quentin . . 8 Huang Yen-Hua H. . 9 Craik David J. . stop_ _Journal_abbreviation 'J. Biol. Chem.' _Journal_name_full 'The Journal of biological chemistry' _Journal_volume 295 _Journal_issue 32 _Journal_ISSN 1083-351X _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 10911 _Page_last 10925 _Year 2020 _Details . save_ ################################## # Molecular system description # ################################## save_assembly_1 _Saveframe_category molecular_system _Mol_system_name 'hyen D' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'hyen D' $entity_1_hyen_D 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_1_hyen_D _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1_hyen_D _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details 'backbone cyclic' ############################## # Polymer residue sequence # ############################## _Residue_count 30 _Mol_residue_sequence ; GFPCGESCVYIPCFTAAIGC SCKSKVCYKN ; loop_ _Residue_seq_code _Residue_label 1 GLY 2 PHE 3 PRO 4 CYS 5 GLY 6 GLU 7 SER 8 CYS 9 VAL 10 TYR 11 ILE 12 PRO 13 CYS 14 PHE 15 THR 16 ALA 17 ALA 18 ILE 19 GLY 20 CYS 21 SER 22 CYS 23 LYS 24 SER 25 LYS 26 VAL 27 CYS 28 TYR 29 LYS 30 ASN stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ #################### # Natural source # #################### save_natural_source_1 _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $entity_1_hyen_D 'Hybanthus enneaspermus' 212266 Eukaryota Viridiplantae Hybanthus enneaspermus stop_ save_ ######################### # Experimental source # ######################### save_experimental_source_1 _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name $entity_1_hyen_D 'purified from the natural source' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1_hyen_D _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1_hyen_D 2 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1_CcpNMR _Saveframe_category software _Name CcpNMR _Version . loop_ _Vendor _Address _Electronic_address CCPN . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1_600 _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_hyen_D save_ save_2D_1H-15N_HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1_hyen_D save_ save_2D_1H-1H_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1_hyen_D save_ save_2D_1H-13C_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_1_hyen_D save_ ####################### # Sample conditions # ####################### save_sample_conditions_1_hyen_D _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0 . M pH 3.5 . pH pressure 1 . atm temperature 298 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_shift_reference_1_DSS _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 C 13 'methyl protons' ppm 0 internal indirect . . . 0.251449530 DSS H 1 'methyl protons' ppm 0 internal direct . . . 1 DSS N 15 'methyl protons' ppm 0 internal 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_assigned_chemical_shifts_1_hyen_D _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H TOCSY' '2D 1H-15N HSQC' '2D 1H-1H NOESY' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_1_hyen_D stop_ _Sample_conditions_label $sample_conditions_1_hyen_D _Chem_shift_reference_set_label $chem_shift_reference_1_DSS _Mol_system_component_name 'hyen D' _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 8.612 . . 2 1 1 GLY HA2 H 4.030 . . 3 1 1 GLY HA3 H 3.446 . . 4 1 1 GLY CA C 45.103 . . 5 1 1 GLY N N 102.336 . . 6 2 2 PHE H H 8.219 . . 7 2 2 PHE HA H 5.177 . . 8 2 2 PHE HB2 H 3.239 . . 9 2 2 PHE HB3 H 3.042 . . 10 2 2 PHE HD1 H 7.393 . . 11 2 2 PHE HD2 H 7.393 . . 12 2 2 PHE HE1 H 7.429 . . 13 2 2 PHE HE2 H 7.429 . . 14 2 2 PHE CA C 55.388 . . 15 2 2 PHE CB C 40.545 . . 16 2 2 PHE N N 121.334 . . 17 3 3 PRO HA H 4.119 . . 18 3 3 PRO HB2 H 1.878 . . 19 3 3 PRO HB3 H 2.070 . . 20 3 3 PRO HG2 H 1.969 . . 21 3 3 PRO HG3 H 2.106 . . 22 3 3 PRO HD2 H 3.950 . . 23 3 3 PRO HD3 H 3.682 . . 24 3 3 PRO CA C 63.032 . . 25 3 3 PRO CB C 32.142 . . 26 3 3 PRO CG C 27.512 . . 27 3 3 PRO CD C 51.034 . . 28 4 4 CYS H H 8.587 . . 29 4 4 CYS HA H 4.601 . . 30 4 4 CYS HB2 H 3.293 . . 31 4 4 CYS HB3 H 3.103 . . 32 4 4 CYS CA C 55.050 . . 33 4 4 CYS CB C 45.448 . . 34 4 4 CYS N N 119.093 . . 35 5 5 GLY H H 8.803 . . 36 5 5 GLY HA2 H 4.127 . . 37 5 5 GLY HA3 H 3.682 . . 38 5 5 GLY CA C 45.791 . . 39 5 5 GLY N N 109.197 . . 40 6 6 GLU H H 7.772 . . 41 6 6 GLU HA H 4.610 . . 42 6 6 GLU HB2 H 1.849 . . 43 6 6 GLU HB3 H 1.748 . . 44 6 6 GLU HG2 H 2.567 . . 45 6 6 GLU HG3 H 2.452 . . 46 6 6 GLU CA C 56.003 . . 47 6 6 GLU CB C 32.581 . . 48 6 6 GLU CG C 33.627 . . 49 6 6 GLU N N 118.194 . . 50 7 7 SER H H 8.793 . . 51 7 7 SER HA H 4.740 . . 52 7 7 SER HB2 H 4.063 . . 53 7 7 SER HB3 H 3.938 . . 54 7 7 SER CA C 57.340 . . 55 7 7 SER CB C 64.796 . . 56 7 7 SER N N 119.438 . . 57 8 8 CYS H H 8.162 . . 58 8 8 CYS HA H 5.307 . . 59 8 8 CYS HB2 H 3.277 . . 60 8 8 CYS HB3 H 3.186 . . 61 8 8 CYS CA C 55.243 . . 62 8 8 CYS CB C 46.106 . . 63 8 8 CYS N N 119.648 . . 64 9 9 VAL H H 7.963 . . 65 9 9 VAL HA H 3.467 . . 66 9 9 VAL HB H 1.680 . . 67 9 9 VAL HG1 H 0.975 . . 68 9 9 VAL HG2 H 0.324 . . 69 9 9 VAL CA C 66.065 . . 70 9 9 VAL CB C 32.103 . . 71 9 9 VAL CG1 C 22.611 . . 72 9 9 VAL CG2 C 20.625 . . 73 9 9 VAL N N 121.905 . . 74 10 10 TYR H H 8.269 . . 75 10 10 TYR HA H 4.680 . . 76 10 10 TYR HB2 H 3.256 . . 77 10 10 TYR HB3 H 2.812 . . 78 10 10 TYR HD1 H 7.149 . . 79 10 10 TYR HD2 H 7.149 . . 80 10 10 TYR HE1 H 6.831 . . 81 10 10 TYR HE2 H 6.831 . . 82 10 10 TYR CA C 58.020 . . 83 10 10 TYR CB C 40.339 . . 84 10 10 TYR N N 115.184 . . 85 11 11 ILE H H 7.558 . . 86 11 11 ILE HA H 4.675 . . 87 11 11 ILE HB H 1.893 . . 88 11 11 ILE HG12 H 1.453 . . 89 11 11 ILE HG13 H 1.096 . . 90 11 11 ILE HG2 H 1.001 . . 91 11 11 ILE HD1 H 0.908 . . 92 11 11 ILE CA C 58.337 . . 93 11 11 ILE CB C 40.583 . . 94 11 11 ILE CG1 C 26.150 . . 95 11 11 ILE CG2 C 17.890 . . 96 11 11 ILE CD1 C 13.558 . . 97 11 11 ILE N N 118.282 . . 98 12 12 PRO HA H 4.390 . . 99 12 12 PRO HB2 H 2.280 . . 100 12 12 PRO HB3 H 1.570 . . 101 12 12 PRO HG2 H 1.871 . . 102 12 12 PRO HG3 H 1.871 . . 103 12 12 PRO HD2 H 3.750 . . 104 12 12 PRO HD3 H 3.517 . . 105 12 12 PRO CA C 62.264 . . 106 12 12 PRO CB C 32.539 . . 107 12 12 PRO CG C 27.481 . . 108 12 12 PRO CD C 50.926 . . 109 13 13 CYS H H 8.544 . . 110 13 13 CYS HA H 4.241 . . 111 13 13 CYS HB2 H 2.978 . . 112 13 13 CYS HB3 H 2.715 . . 113 13 13 CYS CA C 57.204 . . 114 13 13 CYS CB C 41.194 . . 115 13 13 CYS N N 117.886 . . 116 14 14 PHE HA H 4.538 . . 117 14 14 PHE HB2 H 3.353 . . 118 14 14 PHE HB3 H 3.198 . . 119 14 14 PHE HD1 H 7.333 . . 120 14 14 PHE HD2 H 7.333 . . 121 14 14 PHE HE1 H 7.392 . . 122 14 14 PHE HE2 H 7.392 . . 123 14 14 PHE CA C 60.086 . . 124 14 14 PHE CB C 38.269 . . 125 15 15 THR HA H 4.133 . . 126 15 15 THR HB H 4.480 . . 127 15 15 THR HG2 H 1.220 . . 128 15 15 THR CA C 63.833 . . 129 15 15 THR CB C 69.057 . . 130 15 15 THR CG2 C 21.937 . . 131 16 16 ALA H H 7.683 . . 132 16 16 ALA HA H 4.580 . . 133 16 16 ALA HB H 1.416 . . 134 16 16 ALA CA C 54.122 . . 135 16 16 ALA CB C 18.971 . . 136 16 16 ALA N N 126.599 . . 137 17 17 ALA H H 7.920 . . 138 17 17 ALA HA H 4.313 . . 139 17 17 ALA HB H 1.408 . . 140 17 17 ALA CA C 53.222 . . 141 17 17 ALA N N 120.875 . . 142 18 18 ILE H H 7.632 . . 143 18 18 ILE HA H 4.256 . . 144 18 18 ILE HB H 2.040 . . 145 18 18 ILE HG12 H 1.545 . . 146 18 18 ILE HG13 H 1.169 . . 147 18 18 ILE HG2 H 0.904 . . 148 18 18 ILE CA C 61.750 . . 149 18 18 ILE CB C 38.103 . . 150 18 18 ILE CG1 C 27.907 . . 151 18 18 ILE CG2 C 17.468 . . 152 19 19 GLY H H 8.246 . . 153 19 19 GLY HA2 H 4.258 . . 154 19 19 GLY HA3 H 3.790 . . 155 19 19 GLY CA C 45.411 . . 156 19 19 GLY N N 107.416 . . 157 20 20 CYS H H 8.005 . . 158 20 20 CYS HA H 5.019 . . 159 20 20 CYS HB2 H 3.563 . . 160 20 20 CYS HB3 H 2.568 . . 161 20 20 CYS CA C 57.731 . . 162 20 20 CYS CB C 48.378 . . 163 20 20 CYS N N 118.274 . . 164 21 21 SER H H 9.523 . . 165 21 21 SER HA H 4.739 . . 166 21 21 SER HB2 H 3.858 . . 167 21 21 SER HB3 H 3.858 . . 168 21 21 SER CA C 57.352 . . 169 21 21 SER CB C 65.798 . . 170 21 21 SER N N 116.283 . . 171 22 22 CYS H H 8.893 . . 172 22 22 CYS HA H 4.687 . . 173 22 22 CYS HB2 H 3.181 . . 174 22 22 CYS HB3 H 3.105 . . 175 22 22 CYS CA C 56.430 . . 176 22 22 CYS CB C 41.433 . . 177 22 22 CYS N N 124.171 . . 178 23 23 LYS H H 9.579 . . 179 23 23 LYS HA H 4.620 . . 180 23 23 LYS HB2 H 1.825 . . 181 23 23 LYS HB3 H 1.825 . . 182 23 23 LYS HG2 H 1.400 . . 183 23 23 LYS HG3 H 1.267 . . 184 23 23 LYS HD2 H 1.489 . . 185 23 23 LYS HD3 H 1.403 . . 186 23 23 LYS HE2 H 2.777 . . 187 23 23 LYS HE3 H 2.777 . . 188 23 23 LYS HZ H 7.365 . . 189 23 23 LYS CA C 56.868 . . 190 23 23 LYS CB C 34.224 . . 191 23 23 LYS CG C 24.501 . . 192 23 23 LYS CD C 29.075 . . 193 23 23 LYS CE C 42.047 . . 194 23 23 LYS N N 133.445 . . 195 24 24 SER H H 9.287 . . 196 24 24 SER HA H 3.937 . . 197 24 24 SER HB2 H 3.869 . . 198 24 24 SER HB3 H 4.081 . . 199 24 24 SER CA C 58.941 . . 200 24 24 SER CB C 61.928 . . 201 24 24 SER N N 122.132 . . 202 25 25 LYS H H 8.236 . . 203 25 25 LYS HA H 3.523 . . 204 25 25 LYS HB2 H 2.280 . . 205 25 25 LYS HB3 H 1.934 . . 206 25 25 LYS HG2 H 1.298 . . 207 25 25 LYS HG3 H 1.298 . . 208 25 25 LYS HD2 H 1.607 . . 209 25 25 LYS HD3 H 1.669 . . 210 25 25 LYS HE2 H 2.955 . . 211 25 25 LYS HE3 H 2.955 . . 212 25 25 LYS HZ H 7.538 . . 213 25 25 LYS CA C 59.771 . . 214 25 25 LYS CB C 29.891 . . 215 25 25 LYS CG C 25.810 . . 216 25 25 LYS CD C 29.627 . . 217 25 25 LYS CE C 42.378 . . 218 26 26 VAL H H 8.027 . . 219 26 26 VAL HA H 4.286 . . 220 26 26 VAL HB H 2.056 . . 221 26 26 VAL HG1 H 0.959 . . 222 26 26 VAL HG2 H 0.624 . . 223 26 26 VAL CA C 62.166 . . 224 26 26 VAL CB C 35.542 . . 225 26 26 VAL CG1 C 21.967 . . 226 26 26 VAL CG2 C 22.041 . . 227 26 26 VAL N N 124.425 . . 228 27 27 CYS H H 7.982 . . 229 27 27 CYS HA H 5.093 . . 230 27 27 CYS HB2 H 3.032 . . 231 27 27 CYS HB3 H 2.726 . . 232 27 27 CYS CA C 55.831 . . 233 27 27 CYS CB C 43.174 . . 234 27 27 CYS N N 122.985 . . 235 28 28 TYR H H 9.777 . . 236 28 28 TYR HA H 5.215 . . 237 28 28 TYR HB2 H 2.833 . . 238 28 28 TYR HB3 H 2.833 . . 239 28 28 TYR HE1 H 6.831 . . 240 28 28 TYR HE2 H 6.831 . . 241 28 28 TYR CA C 58.670 . . 242 28 28 TYR CB C 45.279 . . 243 28 28 TYR N N 126.823 . . 244 29 29 LYS H H 9.358 . . 245 29 29 LYS HA H 4.655 . . 246 29 29 LYS HB2 H 1.946 . . 247 29 29 LYS HB3 H 1.947 . . 248 29 29 LYS HG2 H 1.256 . . 249 29 29 LYS HG3 H 1.414 . . 250 29 29 LYS HD2 H 1.730 . . 251 29 29 LYS HD3 H 1.665 . . 252 29 29 LYS HE2 H 3.005 . . 253 29 29 LYS HE3 H 3.005 . . 254 29 29 LYS HZ H 7.577 . . 255 29 29 LYS CA C 56.389 . . 256 29 29 LYS CB C 35.211 . . 257 29 29 LYS CG C 25.016 . . 258 29 29 LYS CD C 29.719 . . 259 29 29 LYS CE C 42.315 . . 260 29 29 LYS N N 122.035 . . 261 30 30 ASN H H 9.692 . . 262 30 30 ASN HA H 4.416 . . 263 30 30 ASN HB2 H 3.222 . . 264 30 30 ASN HB3 H 2.957 . . 265 30 30 ASN HD21 H 7.044 . . 266 30 30 ASN HD22 H 7.783 . . 267 30 30 ASN CA C 54.676 . . 268 30 30 ASN CB C 37.602 . . 269 30 30 ASN N N 127.305 . . 270 30 30 ASN ND2 N 112.861 . . stop_ save_