data_50567 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Structure of PCSK9 antagonist P9-38 ; _BMRB_accession_number 50567 _BMRB_flat_file_name bmr50567.str _Entry_type original _Submission_date 2020-11-11 _Accession_date 2020-11-11 _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 Tombling Benjamin J. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 123 "13C chemical shifts" 54 "15N chemical shifts" 21 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2020-11-24 original BMRB . stop_ _Original_release_date 2020-11-12 save_ ############################# # Citation for this entry # ############################# save_citations_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; Bioactive cyclization optimizes the affinity of a proprotein convertase subtilisin/kexin type 9 (PCSK9) peptide inhibitor ; _Citation_status submitted _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 Tombling Benjamin J. . stop_ _Journal_abbreviation 'J. Med. 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_1 _Saveframe_category molecular_system _Mol_system_name P9-38 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label P9-38 $entity_1 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 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1 _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 22 _Mol_residue_sequence ; CTVFTSWEEYLDWNNLHPRN SC ; loop_ _Residue_seq_code _Residue_label 1 CYS 2 THR 3 VAL 4 PHE 5 THR 6 SER 7 TRP 8 GLU 9 GLU 10 TYR 11 LEU 12 ASP 13 TRP 14 ASN 15 ASN 16 LEU 17 HIS 18 PRO 19 ARG 20 ASN 21 SER 22 CYS 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 . . . . . . 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_type _Vector_name $entity_1 'recombinant technology' . Escherichia coli . plasmid pComb3 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 $entity_1 0.75 mM 0.5 1 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name CcpNMR _Version . loop_ _Task 'chemical shift assignment' 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_1H_1 _Saveframe_category NMR_applied_experiment _Experiment_name '1D 1H' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_2D_1H-13C_HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-1H_COSY_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H 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 pH 3.25 0.25 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 DSS C 13 'methyl protons' ppm 0 internal indirect . . . 0.25144953 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 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_1 stop_ loop_ _Experiment_label '1D 1H' '2D 1H-15N HSQC' '2D 1H-13C HSQC' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '2D 1H-1H COSY' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name P9-38 _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 CYS HA H 4.289 0.000 1 2 1 1 CYS HB2 H 2.995 0.000 1 3 1 1 CYS HB3 H 3.239 0.000 1 4 2 2 THR H H 8.281 0.000 1 5 2 2 THR HA H 4.165 0.000 1 6 2 2 THR HB H 3.580 0.000 1 7 2 2 THR HG2 H 0.694 0.000 1 8 2 2 THR CA C 61.935 0.000 1 9 2 2 THR CB C 69.946 0.000 1 10 2 2 THR CG2 C 21.206 0.000 1 11 3 3 VAL H H 8.139 0.000 1 12 3 3 VAL HA H 3.925 0.000 1 13 3 3 VAL HB H 1.907 0.000 1 14 3 3 VAL HG1 H 0.867 0.000 1 15 3 3 VAL HG2 H 0.867 0.000 1 16 3 3 VAL CA C 62.277 0.000 1 17 3 3 VAL CB C 32.363 0.000 1 18 3 3 VAL CG1 C 21.002 0.000 1 19 3 3 VAL CG2 C 21.002 0.000 1 20 3 3 VAL N N 124.083 0.000 1 21 4 4 PHE H H 8.305 0.000 1 22 4 4 PHE HA H 4.750 0.000 1 23 4 4 PHE HB2 H 3.273 0.000 1 24 4 4 PHE HB3 H 2.838 0.000 1 25 4 4 PHE HD1 H 7.187 0.000 1 26 4 4 PHE HD2 H 7.187 0.000 1 27 4 4 PHE CB C 40.562 0.000 1 28 4 4 PHE N N 126.214 0.000 1 29 5 5 THR H H 8.609 0.000 1 30 5 5 THR HA H 4.461 0.000 1 31 5 5 THR HB H 4.443 0.000 1 32 5 5 THR HG2 H 1.246 0.000 1 33 5 5 THR CA C 62.142 0.000 1 34 5 5 THR CB C 69.701 0.000 1 35 5 5 THR CG2 C 21.868 0.000 1 36 6 6 SER H H 7.708 0.000 1 37 6 6 SER HA H 4.281 0.000 1 38 6 6 SER HB2 H 3.994 0.000 1 39 6 6 SER HB3 H 3.894 0.000 1 40 6 6 SER CA C 54.578 0.000 1 41 6 6 SER CB C 65.449 0.000 1 42 7 7 TRP H H 8.284 0.000 1 43 7 7 TRP HA H 4.554 0.000 1 44 7 7 TRP HB2 H 3.163 0.000 1 45 7 7 TRP HB3 H 3.086 0.000 1 46 7 7 TRP HD1 H 7.212 0.000 1 47 7 7 TRP HE1 H 10.207 0.000 1 48 7 7 TRP CA C 58.709 0.000 1 49 7 7 TRP CB C 30.144 0.000 1 50 7 7 TRP NE1 N 129.191 0.000 1 51 8 8 GLU H H 8.250 0.000 1 52 8 8 GLU HA H 3.756 0.000 1 53 8 8 GLU HB2 H 1.945 0.000 1 54 8 8 GLU HB3 H 1.878 0.000 1 55 8 8 GLU HG2 H 2.349 0.000 1 56 8 8 GLU HG3 H 2.267 0.000 1 57 8 8 GLU CA C 58.736 0.000 1 58 8 8 GLU CB C 27.917 0.000 1 59 8 8 GLU CG C 33.412 0.000 1 60 8 8 GLU N N 117.745 0.000 1 61 9 9 GLU H H 7.627 0.000 1 62 9 9 GLU HA H 4.004 0.000 1 63 9 9 GLU HB2 H 2.168 0.000 1 64 9 9 GLU HB3 H 2.114 0.000 1 65 9 9 GLU HG2 H 2.548 0.000 1 66 9 9 GLU HG3 H 2.411 0.000 1 67 9 9 GLU CA C 58.408 0.000 1 68 9 9 GLU CB C 28.620 0.000 1 69 9 9 GLU CG C 33.667 0.000 1 70 9 9 GLU N N 118.252 0.000 1 71 10 10 TYR H H 7.508 0.000 1 72 10 10 TYR HA H 3.417 0.000 1 73 10 10 TYR HB2 H 2.966 0.000 1 74 10 10 TYR HB3 H 2.625 0.000 1 75 10 10 TYR HD1 H 6.548 0.000 1 76 10 10 TYR HD2 H 6.548 0.000 1 77 10 10 TYR CB C 37.754 0.000 1 78 10 10 TYR N N 120.593 0.000 1 79 11 11 LEU H H 8.068 0.000 1 80 11 11 LEU HA H 3.616 0.000 1 81 11 11 LEU HB2 H 1.416 0.000 1 82 11 11 LEU HB3 H 1.210 0.000 1 83 11 11 LEU HG H 0.992 0.000 1 84 11 11 LEU HD1 H 0.622 0.000 1 85 11 11 LEU HD2 H 0.611 0.000 1 86 11 11 LEU CA C 57.122 0.000 1 87 11 11 LEU CB C 41.676 0.000 1 88 11 11 LEU CG C 26.135 0.000 1 89 11 11 LEU CD1 C 24.897 0.000 1 90 11 11 LEU CD2 C 22.694 0.000 1 91 12 12 ASP H H 8.160 0.000 1 92 12 12 ASP HA H 4.389 0.000 1 93 12 12 ASP HB2 H 2.817 0.000 1 94 12 12 ASP HB3 H 2.817 0.000 1 95 12 12 ASP CB C 38.368 0.000 1 96 12 12 ASP N N 117.854 0.000 1 97 13 13 TRP H H 8.058 0.000 1 98 13 13 TRP HA H 4.223 0.000 1 99 13 13 TRP HB2 H 3.157 0.000 1 100 13 13 TRP HB3 H 3.335 0.000 1 101 13 13 TRP HD1 H 7.304 0.000 1 102 13 13 TRP HE1 H 10.045 0.000 1 103 13 13 TRP CA C 61.112 0.000 1 104 13 13 TRP CB C 29.441 0.000 1 105 13 13 TRP N N 120.700 0.000 1 106 13 13 TRP NE1 N 129.620 0.000 1 107 14 14 ASN H H 8.228 0.000 1 108 14 14 ASN HA H 4.189 0.000 1 109 14 14 ASN HB2 H 2.506 0.000 1 110 14 14 ASN HB3 H 2.427 0.000 1 111 14 14 ASN HD21 H 7.157 0.000 1 112 14 14 ASN HD22 H 6.284 0.000 1 113 14 14 ASN CA C 55.778 0.000 1 114 14 14 ASN CB C 38.275 0.000 1 115 14 14 ASN N N 118.712 0.000 1 116 14 14 ASN ND2 N 111.695 0.000 1 117 15 15 ASN H H 7.979 0.000 1 118 15 15 ASN HA H 4.388 0.000 1 119 15 15 ASN HB2 H 2.730 0.000 1 120 15 15 ASN HB3 H 2.750 0.000 1 121 15 15 ASN HD21 H 7.531 0.000 1 122 15 15 ASN HD22 H 6.800 0.000 1 123 15 15 ASN CA C 55.186 0.000 1 124 15 15 ASN CB C 38.464 0.000 1 125 15 15 ASN N N 117.434 0.000 1 126 15 15 ASN ND2 N 112.187 0.000 1 127 16 16 LEU H H 7.389 0.000 1 128 16 16 LEU HA H 4.084 0.000 1 129 16 16 LEU HB2 H 1.358 0.000 1 130 16 16 LEU HB3 H 1.069 0.000 1 131 16 16 LEU HG H 1.465 0.000 1 132 16 16 LEU HD1 H 0.792 0.000 1 133 16 16 LEU HD2 H 0.729 0.000 1 134 16 16 LEU CA C 55.282 0.000 1 135 16 16 LEU CB C 42.871 0.000 1 136 16 16 LEU CG C 26.931 0.000 1 137 16 16 LEU CD1 C 24.884 0.000 1 138 16 16 LEU CD2 C 22.831 0.000 1 139 16 16 LEU N N 117.967 0.000 1 140 17 17 HIS H H 7.549 0.000 1 141 17 17 HIS HA H 4.750 0.000 1 142 17 17 HIS HB2 H 3.294 0.000 1 143 17 17 HIS HB3 H 3.405 0.000 1 144 17 17 HIS CB C 27.771 0.000 1 145 17 17 HIS N N 116.543 0.000 1 146 18 18 PRO HA H 4.408 0.000 1 147 18 18 PRO HB2 H 2.261 0.000 1 148 18 18 PRO HB3 H 1.879 0.000 1 149 18 18 PRO HG2 H 1.901 0.000 1 150 18 18 PRO HG3 H 1.901 0.000 1 151 18 18 PRO HD2 H 3.406 0.000 1 152 18 18 PRO HD3 H 3.297 0.000 1 153 18 18 PRO CA C 63.922 0.000 1 154 18 18 PRO CB C 32.079 0.000 1 155 18 18 PRO CG C 27.409 0.000 1 156 18 18 PRO CD C 50.306 0.000 1 157 19 19 ARG H H 8.613 0.000 1 158 19 19 ARG HA H 4.206 0.000 1 159 19 19 ARG HB2 H 1.910 0.000 1 160 19 19 ARG HB3 H 1.789 0.000 1 161 19 19 ARG HG2 H 1.565 0.000 1 162 19 19 ARG HG3 H 1.565 0.000 1 163 19 19 ARG HD2 H 3.154 0.000 1 164 19 19 ARG HD3 H 3.154 0.000 1 165 19 19 ARG HH11 H 7.393 0.000 1 166 19 19 ARG HH12 H 7.393 0.000 1 167 19 19 ARG HH21 H 7.812 0.000 1 168 19 19 ARG HH22 H 7.812 0.000 1 169 19 19 ARG CA C 56.523 0.000 1 170 19 19 ARG CB C 29.379 0.000 1 171 19 19 ARG CG C 27.460 0.000 1 172 19 19 ARG CD C 43.287 0.000 1 173 19 19 ARG NH1 N 108.464 0.000 1 174 19 19 ARG NH2 N 108.450 0.000 1 175 20 20 ASN H H 8.086 0.000 1 176 20 20 ASN HA H 4.832 0.000 1 177 20 20 ASN HB2 H 2.924 0.000 1 178 20 20 ASN HB3 H 2.785 0.000 1 179 20 20 ASN HD21 H 7.893 0.000 1 180 20 20 ASN HD22 H 7.099 0.000 1 181 20 20 ASN CA C 53.177 0.000 1 182 20 20 ASN CB C 40.278 0.000 1 183 20 20 ASN N N 119.106 0.000 1 184 20 20 ASN ND2 N 113.924 0.000 1 185 21 21 SER H H 8.623 0.000 1 186 21 21 SER HA H 4.539 0.000 1 187 21 21 SER HB2 H 3.967 0.000 1 188 21 21 SER HB3 H 3.939 0.000 1 189 21 21 SER CA C 59.468 0.000 1 190 21 21 SER CB C 63.768 0.000 1 191 21 21 SER N N 118.444 0.000 1 192 22 22 CYS H H 8.952 0.000 1 193 22 22 CYS HA H 4.842 0.000 1 194 22 22 CYS HB2 H 3.426 0.000 1 195 22 22 CYS HB3 H 3.024 0.000 1 196 22 22 CYS CA C 55.402 0.000 1 197 22 22 CYS CB C 41.218 0.000 1 198 22 22 CYS N N 120.950 0.000 1 stop_ save_