data_26677 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H, 13C, and 15N Chemical Shift Assignments for redox-stable cyclic peptide inhibitors of SPSB2-iNOS interaction - CP2 ; _BMRB_accession_number 26677 _BMRB_flat_file_name bmr26677.str _Entry_type original _Submission_date 2015-10-03 _Accession_date 2015-10-03 _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 Yap 'Beow Keat' . . 2 Norton Raymond . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 43 "13C chemical shifts" 22 "15N chemical shifts" 11 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2016-09-09 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 26676 CP1 stop_ _Original_release_date 2016-09-09 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Redox-stable cyclic peptide inhibitors of the SPSB2-iNOS interaction ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 26921848 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Yap 'Beow Keat' . . 2 Harjani J. R. . 3 Leung E. W. . 4 Nicholson S. E. . 5 Scanlon M. J. . 6 Chalmers D. K. . 7 Thompson P. E. . 8 Baell J. B. . 9 Norton Raymond . . stop_ _Journal_abbreviation 'FEBS Lett.' _Journal_volume 590 _Journal_issue 6 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 696 _Page_last 704 _Year 2016 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name CP2 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label WDINNNX $WDINNNX stop_ _System_molecular_weight 827.55 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details 'Cyclic peptide c[WDINNNbA]' save_ ######################## # Monomeric polymers # ######################## save_WDINNNX _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common WDINNNX _Molecular_mass . _Mol_thiol_state 'not present' _Details 'BAL is residue number 7 of CP2' ############################## # Polymer residue sequence # ############################## _Residue_count 7 _Mol_residue_sequence ; WDINNNX ; loop_ _Residue_seq_code _Residue_label 1 TRP 2 ASP 3 ILE 4 ASN 5 ASN 6 ASN 7 BAL stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_BAL _Saveframe_category polymer_residue _Mol_type PEPTIDE-LIKE _Name_common BETA-ALANINE _BMRB_code BAL _PDB_code BAL _Standard_residue_derivative . _Molecular_mass 89.093 _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 . ? CB CB C . 0 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HB3 HB3 H . 0 . ? HB2 HB2 H . 0 . ? HA1 HA1 H . 0 . ? HA2 HA2 H . 0 . ? HXT HXT 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 CB ? ? SING N H ? ? SING N H2 ? ? SING CB CA ? ? SING CB HB3 ? ? SING CB HB2 ? ? SING CA C ? ? SING CA HA1 ? ? SING CA HA2 ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Details $WDINNNX . . . . . . 'Synthesized by Fmoc-based solid phase peptide synthesis' 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 $WDINNNX 'chemical synthesis' . . . . . 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 $WDINNNX 1.9 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CcpNmr_Analysis _Saveframe_category software _Name CcpNmr_Analysis _Version 2.1.5 loop_ _Vendor _Address _Electronic_address CCPN . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version 3.2 loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_AV600 _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 save_ save_2D_1H-1H_ROESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H ROESY' _Sample_label $sample_1 save_ save_2D_DQF-COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _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_2D_1H-13C_HSQC_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_H2O _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 4.8 . pH temperature 298 . K stop_ save_ save_sample_conditions_D2O _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH* 4.8 . pH* 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 C 13 'methyl protons' ppm 0.00 na indirect . . . 0.251449530 DSS H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 DSS N 15 'methyl protons' ppm 0.00 na 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_chem_shift_list_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H TOCSY' '2D 1H-1H ROESY' '2D DQF-COSY' '2D 1H-15N HSQC' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_H2O _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name WDINNNX _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 TRP H H 8.106 0.001 1 2 1 1 TRP HA H 4.703 0.010 1 3 1 1 TRP HB2 H 3.263 0.005 2 4 1 1 TRP HB3 H 3.361 0.007 2 5 1 1 TRP HD1 H 7.279 0.005 1 6 1 1 TRP HE1 H 10.120 0.001 1 7 1 1 TRP HE3 H 7.659 0.007 1 8 1 1 TRP HZ2 H 7.507 0.007 1 9 1 1 TRP HZ3 H 7.185 0.007 1 10 1 1 TRP HH2 H 7.255 0.007 1 11 1 1 TRP CA C 55.180 0.000 1 12 1 1 TRP CB C 26.477 0.002 1 13 1 1 TRP CD1 C 124.426 0.000 1 14 1 1 TRP CE3 C 118.402 0.000 1 15 1 1 TRP CZ2 C 111.983 0.000 1 16 1 1 TRP CZ3 C 119.449 0.000 1 17 1 1 TRP CH2 C 122.063 0.000 1 18 1 1 TRP N N 125.716 0.000 1 19 1 1 TRP NE1 N 129.249 0.000 1 20 2 2 ASP H H 8.133 0.006 1 21 2 2 ASP HA H 4.652 0.006 1 22 2 2 ASP HB3 H 2.650 0.004 1 23 2 2 ASP CA C 50.829 0.000 1 24 2 2 ASP CB C 38.954 0.000 1 25 2 2 ASP N N 119.487 0.000 1 26 3 3 ILE H H 8.250 0.005 1 27 3 3 ILE HA H 4.057 0.004 1 28 3 3 ILE HB H 1.905 0.006 1 29 3 3 ILE HG12 H 1.246 0.011 2 30 3 3 ILE HG13 H 1.439 0.011 2 31 3 3 ILE HG2 H 0.933 0.010 1 32 3 3 ILE HD1 H 0.900 0.006 1 33 3 3 ILE CA C 60.308 0.000 1 34 3 3 ILE CB C 35.780 0.000 1 35 3 3 ILE CG1 C 24.890 0.006 1 36 3 3 ILE CG2 C 14.802 0.000 1 37 3 3 ILE CD1 C 10.893 0.000 1 38 3 3 ILE N N 119.799 0.000 1 39 4 4 ASN H H 8.186 0.004 1 40 4 4 ASN HA H 4.676 0.010 1 41 4 4 ASN HB2 H 2.757 0.004 2 42 4 4 ASN HB3 H 2.870 0.012 2 43 4 4 ASN HD21 H 6.927 0.001 1 44 4 4 ASN HD22 H 7.715 0.001 1 45 4 4 ASN CA C 51.215 0.000 1 46 4 4 ASN CB C 35.930 0.003 1 47 4 4 ASN N N 118.232 0.000 1 48 4 4 ASN ND2 N 113.708 0.008 1 49 5 5 ASN H H 8.011 0.005 1 50 5 5 ASN HA H 4.601 0.005 1 51 5 5 ASN HB2 H 2.671 0.007 2 52 5 5 ASN HB3 H 2.838 0.004 2 53 5 5 ASN HD21 H 6.735 0.001 1 54 5 5 ASN HD22 H 7.656 0.003 1 55 5 5 ASN CA C 51.044 0.000 1 56 5 5 ASN CB C 35.768 0.014 1 57 5 5 ASN N N 115.738 0.000 1 58 5 5 ASN ND2 N 113.218 0.017 1 59 6 6 ASN H H 8.304 0.002 1 60 6 6 ASN HA H 4.564 0.006 1 61 6 6 ASN HB2 H 2.660 0.001 2 62 6 6 ASN HB3 H 2.795 0.004 2 63 6 6 ASN HD21 H 6.809 0.001 1 64 6 6 ASN HD22 H 7.580 0.000 1 65 6 6 ASN CA C 51.353 0.000 1 66 6 6 ASN CB C 35.902 0.000 1 67 6 6 ASN N N 117.565 0.000 1 68 6 6 ASN ND2 N 112.642 0.006 1 69 7 7 BAL H H 7.901 0.002 1 70 7 7 BAL HA1 H 2.431 0.007 2 71 7 7 BAL HA2 H 2.292 0.009 2 72 7 7 BAL HB2 H 3.481 0.004 2 73 7 7 BAL HB3 H 3.317 0.005 2 74 7 7 BAL CA C 34.968 0.005 1 75 7 7 BAL CB C 35.920 0.005 1 76 7 7 BAL N N 116.672 0.000 1 stop_ save_