data_26676 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H, 13C, and 15N Chemical Shift Assignments for the redox-stable inhibitor of SPSB2-iNOS interaction - CP1 ; _BMRB_accession_number 26676 _BMRB_flat_file_name bmr26676.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" 48 "13C chemical shifts" 23 "15N chemical shifts" 12 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2016-09-09 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 26677 CP2 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 CP1 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label XVDINNN $XVDINNN stop_ _System_molecular_weight 914.60 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details 'Cyclic peptide c[(CST)VDINNN]' save_ ######################## # Monomeric polymers # ######################## save_XVDINNN _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common XVDINNN _Molecular_mass . _Mol_thiol_state 'not present' _Details ; CST as residue 1 of CP1. Formula: C9 H17 N3 O4 S. Formula_weight: 263.31 Designation of each corresponding atoms of CST are shown in the image file highlighted in purple. ; ############################## # Polymer residue sequence # ############################## _Residue_count 7 _Mol_residue_sequence ; XVDINNN ; loop_ _Residue_seq_code _Residue_label 1 CST-2 2 VAL 3 ASP 4 ILE 5 ASN 6 ASN 7 ASN 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 _Details $XVDINNN . . . . . . 'Synthesized using Fmoc-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 $XVDINNN '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 $XVDINNN 700 uM '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_CP1_conditions _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 4.8 . pH temperature 283 . K stop_ save_ save_CP1_in_D2O _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH* 4.8 . pH* temperature 283 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift _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_ _Software_label $CcpNmr_Analysis stop_ 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 $CP1_conditions _Chem_shift_reference_set_label $chemical_shift _Mol_system_component_name XVDINNN _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 CST-2 H H 8.437 0.008 1 2 1 1 CST-2 HA H 4.470 0.006 1 3 1 1 CST-2 HB2 H 3.005 0.006 2 4 1 1 CST-2 HB3 H 2.944 0.004 2 5 1 1 CST-2 HD1 H 2.626 0.007 1 6 1 1 CST-2 HE1 H 2.025 0.010 2 7 1 1 CST-2 HE2 H 1.959 0.004 2 8 1 1 CST-2 HZ H 4.429 0.010 1 9 1 1 CST-2 HH11 H 8.419 0.003 1 10 1 1 CST-2 HH21 H 7.763 0.001 1 11 1 1 CST-2 HH22 H 7.279 0.001 1 12 1 1 CST-2 HI1 H 2.007 0.003 1 13 1 1 CST-2 HI2 H 2.007 0.003 1 14 1 1 CST-2 HI3 H 2.007 0.003 1 15 1 1 CST-2 CA C 53.065 0.000 1 16 1 1 CST-2 CB C 32.038 0.000 1 17 1 1 CST-2 CD C 27.406 0.000 1 18 1 1 CST-2 CE C 30.675 0.005 1 19 1 1 CST-2 CZ C 52.890 0.000 1 20 1 1 CST-2 CI1 C 21.508 0.000 1 21 1 1 CST-2 N N 120.536 0.000 1 22 1 1 CST-2 NH1 N 126.674 0.000 1 23 1 1 CST-2 NH2 N 109.438 0.002 1 24 2 2 VAL H H 8.428 0.003 1 25 2 2 VAL HA H 4.070 0.003 1 26 2 2 VAL HB H 2.117 0.007 1 27 2 2 VAL HG1 H 0.958 0.004 2 28 2 2 VAL HG2 H 0.944 0.007 2 29 2 2 VAL CA C 60.438 0.000 1 30 2 2 VAL CB C 29.768 0.000 1 31 2 2 VAL CG1 C 17.733 0.000 2 32 2 2 VAL CG2 C 18.409 0.000 2 33 2 2 VAL N N 122.081 0.000 1 34 3 3 ASP H H 8.168 0.002 1 35 3 3 ASP HA H 4.698 0.003 1 36 3 3 ASP HB2 H 2.763 0.003 2 37 3 3 ASP HB3 H 2.596 0.010 2 38 3 3 ASP CA C 50.856 0.000 1 39 3 3 ASP CB C 39.273 0.000 1 40 3 3 ASP N N 122.050 0.000 1 41 4 4 ILE H H 8.386 0.010 1 42 4 4 ILE HA H 4.125 0.011 1 43 4 4 ILE HB H 1.947 0.005 1 44 4 4 ILE HG12 H 1.422 0.010 2 45 4 4 ILE HG13 H 1.242 0.012 2 46 4 4 ILE HG2 H 0.931 0.021 1 47 4 4 ILE HD1 H 0.896 0.006 1 48 4 4 ILE CA C 59.810 0.000 1 49 4 4 ILE CB C 35.647 0.000 1 50 4 4 ILE CG1 C 24.541 0.010 1 51 4 4 ILE CG2 C 14.852 0.000 1 52 4 4 ILE CD1 C 10.893 0.000 1 53 4 4 ILE N N 121.557 0.000 1 54 5 5 ASN H H 8.493 0.004 1 55 5 5 ASN HA H 4.704 0.002 1 56 5 5 ASN HB2 H 2.792 0.008 2 57 5 5 ASN HB3 H 2.890 0.006 2 58 5 5 ASN HD21 H 7.852 0.010 1 59 5 5 ASN HD22 H 6.999 0.001 1 60 5 5 ASN CA C 50.856 0.000 1 61 5 5 ASN CB C 35.970 0.015 1 62 5 5 ASN N N 119.596 0.000 1 63 5 5 ASN ND2 N 114.414 0.003 1 64 6 6 ASN H H 8.095 0.006 1 65 6 6 ASN HA H 4.702 0.001 1 66 6 6 ASN HB2 H 2.745 0.010 2 67 6 6 ASN HB3 H 2.906 0.009 2 68 6 6 ASN HD21 H 6.947 0.001 1 69 6 6 ASN HD22 H 7.677 0.005 1 70 6 6 ASN CA C 50.856 0.000 1 71 6 6 ASN CB C 35.452 0.019 1 72 6 6 ASN N N 117.018 0.000 1 73 6 6 ASN ND2 N 113.021 0.006 1 74 7 7 ASN H H 8.606 0.005 1 75 7 7 ASN HA H 4.699 0.003 1 76 7 7 ASN HB2 H 2.760 0.005 2 77 7 7 ASN HB3 H 2.896 0.002 2 78 7 7 ASN HD21 H 6.947 0.002 1 79 7 7 ASN HD22 H 7.807 0.006 1 80 7 7 ASN CA C 50.856 0.000 1 81 7 7 ASN CB C 36.565 0.001 1 82 7 7 ASN N N 118.272 0.000 1 83 7 7 ASN ND2 N 113.674 0.018 1 stop_ save_