data_30499 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Heterogeneous-Backbone Mimics of a Designed Disulfide-Rich Protein: Aib turn, Aib helix, N-methyl hairpin ; _BMRB_accession_number 30499 _BMRB_flat_file_name bmr30499.str _Entry_type original _Submission_date 2018-07-20 _Accession_date 2018-07-20 _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 Cabalteja C. C. . 2 Mihalko D. S. . 3 Horne W. S. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 157 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2019-05-15 update BMRB 'update entry citation' 2018-11-12 original author 'original release' stop_ _Original_release_date 2018-07-30 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; Heterogeneous-Backbone Foldamer Mimics of a Computationally Designed, Disulfide-Rich Miniprotein ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 30326175 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Cabalteja C. C. . 2 Mihalko D. S. . 3 Horne W. S. . stop_ _Journal_abbreviation Chembiochem. _Journal_volume 20 _Journal_issue 1 _Journal_CSD 0353 _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 103 _Page_last 110 _Year 2019 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Designed peptide NC_HEE_D1: Aib turn, Aib helix, N-methyl hairpin mutant' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label entity_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 3156.709 _Mol_thiol_state 'all disulfide bound' _Details 'disulfide bonds between Cys4-Cys18 and between Cys14-Cys27' ############################## # Polymer residue sequence # ############################## _Residue_count 28 _Mol_residue_sequence ; NDXCKXLKXRYXGCEXRCDX PRYEXHCX ; loop_ _Residue_seq_code _Residue_label 1 ASN 2 ASP 3 AIB 4 CYS 5 LYS 6 AIB 7 LEU 8 LYS 9 AIB 10 ARG 11 TYR 12 AIB 13 GLY 14 CYS 15 GLU 16 MVA 17 ARG 18 CYS 19 ASP 20 DPR 21 PRO 22 ARG 23 TYR 24 GLU 25 MVA 26 HIS 27 CYS 28 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_DPR _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-PROLINE _BMRB_code DPR _PDB_code DPR _Standard_residue_derivative . _Molecular_mass 115.130 _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 . ? CA CA C . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD CD C . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 H . 0 . ? HD2 HD2 H . 0 . ? HD3 HD3 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 CA ? ? SING N CD ? ? SING N H ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD ? ? SING CG HG2 ? ? SING CG HG3 ? ? SING CD HD2 ? ? SING CD HD3 ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? stop_ save_ 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_ save_chem_comp_AIB _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common 'ALPHA-AMINOISOBUTYRIC ACID' _BMRB_code AIB _PDB_code AIB _Standard_residue_derivative . _Molecular_mass 103.120 _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 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? CB1 CB1 C . 0 . ? CB2 CB2 C . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HO2 HO2 H . 0 . ? HB11 HB11 H . 0 . ? HB12 HB12 H . 0 . ? HB13 HB13 H . 0 . ? HB21 HB21 H . 0 . ? HB22 HB22 H . 0 . ? HB23 HB23 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 CA ? ? SING N H ? ? SING N H2 ? ? SING CA C ? ? SING CA CB1 ? ? SING CA CB2 ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HO2 ? ? SING CB1 HB11 ? ? SING CB1 HB12 ? ? SING CB1 HB13 ? ? SING CB2 HB21 ? ? SING CB2 HB22 ? ? SING CB2 HB23 ? ? stop_ save_ save_chem_comp_MVA _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common N-METHYLVALINE _BMRB_code MVA _PDB_code MVA _Standard_residue_derivative . _Molecular_mass 131.173 _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 . ? CN CN C . 0 . ? CA CA C . 0 . ? CB CB C . 0 . ? CG1 CG1 C . 0 . ? CG2 CG2 C . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? HN1 HN1 H . 0 . ? HN2 HN2 H . 0 . ? HN3 HN3 H . 0 . ? HA HA H . 0 . ? HB HB H . 0 . ? HG11 HG11 H . 0 . ? HG12 HG12 H . 0 . ? HG13 HG13 H . 0 . ? HG21 HG21 H . 0 . ? HG22 HG22 H . 0 . ? HG23 HG23 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 CN ? ? SING N CA ? ? SING N H ? ? SING CN HN1 ? ? SING CN HN2 ? ? SING CN HN3 ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB CG1 ? ? SING CB CG2 ? ? SING CB HB ? ? SING CG1 HG11 ? ? SING CG1 HG12 ? ? SING CG1 HG13 ? ? SING CG2 HG21 ? ? SING CG2 HG22 ? ? SING CG2 HG23 ? ? 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 $entity_1 . 32630 . . . . 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 '0.2 mM NA DSS, 1.0 mM NA Designed peptide NC_HEE_D1: Aib turn, Aib helix, N-methyl hairpin mutant, 90% H2O/10% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling DSS 0.2 mM 'natural abundance' $entity_1 1.0 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ save_software_2 _Saveframe_category software _Name ARIA _Version 2.3 loop_ _Vendor _Address _Electronic_address "Linge, O'Donoghue and Nilges" . . stop_ loop_ _Task 'structure calculation' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 700 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_TOCSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D TOCSY' _Sample_label $sample_1 save_ save_2D_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D NOESY' _Sample_label $sample_1 save_ save_2D_COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 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 'ionic strength' 5 . mM pH 4.0 . pH pressure 1 . atm temperature 275 . 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 H 1 'methyl protons' ppm 0.000 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 '2D TOCSY' '2D COSY' '2D NOESY' 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 entity_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 ASN HA H 4.345 0.000 1 2 1 1 ASN HB2 H 3.032 0.000 1 3 1 1 ASN HB3 H 3.032 0.000 1 4 1 1 ASN HD21 H 7.087 0.000 2 5 1 1 ASN HD22 H 7.754 0.000 2 6 2 2 ASP H H 8.811 0.001 1 7 2 2 ASP HA H 4.718 0.000 1 8 2 2 ASP HB2 H 2.866 0.001 2 9 2 2 ASP HB3 H 2.735 0.000 2 10 3 3 AIB H H 8.425 0.001 1 11 3 3 AIB HB11 H 1.440 0.000 2 12 3 3 AIB HB21 H 1.460 0.000 2 13 4 4 CYS H H 8.252 0.001 1 14 4 4 CYS HA H 4.356 0.000 1 15 4 4 CYS HB2 H 3.254 0.000 2 16 4 4 CYS HB3 H 3.150 0.000 2 17 5 5 LYS H H 7.777 0.000 1 18 5 5 LYS HA H 3.917 0.002 1 19 5 5 LYS HB2 H 1.893 0.002 1 20 5 5 LYS HB3 H 1.893 0.002 1 21 5 5 LYS HG2 H 1.537 0.000 2 22 5 5 LYS HG3 H 1.411 0.000 2 23 5 5 LYS HD2 H 1.727 0.001 1 24 5 5 LYS HD3 H 1.727 0.001 1 25 5 5 LYS HE2 H 3.016 0.001 1 26 5 5 LYS HE3 H 3.016 0.001 1 27 6 6 AIB H H 7.909 0.001 1 28 6 6 AIB HB11 H 1.466 0.000 2 29 6 6 AIB HB21 H 1.492 0.000 2 30 7 7 LEU H H 7.507 0.001 1 31 7 7 LEU HA H 4.056 0.000 1 32 7 7 LEU HB2 H 1.712 0.000 2 33 7 7 LEU HB3 H 1.420 0.000 2 34 7 7 LEU HG H 1.535 0.000 1 35 7 7 LEU HD1 H 0.534 0.001 2 36 7 7 LEU HD2 H 0.614 0.000 2 37 8 8 LYS H H 7.877 0.000 1 38 8 8 LYS HA H 3.957 0.001 1 39 8 8 LYS HB2 H 1.872 0.000 1 40 8 8 LYS HB3 H 1.872 0.000 1 41 8 8 LYS HG2 H 1.620 0.001 2 42 8 8 LYS HG3 H 1.412 0.000 2 43 8 8 LYS HD2 H 1.709 0.000 1 44 8 8 LYS HD3 H 1.709 0.000 1 45 8 8 LYS HE2 H 2.984 0.002 1 46 8 8 LYS HE3 H 2.984 0.002 1 47 9 9 AIB H H 7.675 0.000 1 48 9 9 AIB HB11 H 1.482 0.000 1 49 10 10 ARG H H 7.481 0.001 1 50 10 10 ARG HA H 4.050 0.001 1 51 10 10 ARG HB2 H 1.696 0.000 2 52 10 10 ARG HB3 H 1.555 0.001 2 53 10 10 ARG HG2 H 1.319 0.002 2 54 10 10 ARG HG3 H 1.236 0.003 2 55 10 10 ARG HD2 H 2.976 0.003 1 56 10 10 ARG HD3 H 2.976 0.003 1 57 10 10 ARG HE H 7.013 0.001 1 58 11 11 TYR H H 7.791 0.000 1 59 11 11 TYR HA H 4.640 0.001 1 60 11 11 TYR HB2 H 3.075 0.001 2 61 11 11 TYR HB3 H 2.484 0.001 2 62 11 11 TYR HD1 H 7.152 0.000 1 63 11 11 TYR HD2 H 7.152 0.000 1 64 11 11 TYR HE1 H 6.699 0.000 1 65 11 11 TYR HE2 H 6.699 0.000 1 66 12 12 AIB H H 7.551 0.000 1 67 12 12 AIB HB11 H 1.455 0.000 2 68 12 12 AIB HB21 H 1.539 0.000 2 69 13 13 GLY H H 8.462 0.001 1 70 13 13 GLY HA2 H 4.125 0.000 2 71 13 13 GLY HA3 H 3.831 0.000 2 72 14 14 CYS H H 8.021 0.001 1 73 14 14 CYS HA H 5.046 0.000 1 74 14 14 CYS HB2 H 3.433 0.000 2 75 14 14 CYS HB3 H 2.478 0.000 2 76 15 15 GLU H H 8.674 0.001 1 77 15 15 GLU HA H 5.010 0.001 1 78 15 15 GLU HB2 H 2.207 0.002 1 79 15 15 GLU HB3 H 2.207 0.002 1 80 15 15 GLU HG2 H 2.541 0.002 2 81 15 15 GLU HG3 H 2.382 0.000 2 82 16 16 MVA HA H 5.174 0.001 1 83 16 16 MVA HB H 2.138 0.001 1 84 16 16 MVA HG11 H 0.704 0.000 2 85 16 16 MVA HG21 H 0.748 0.000 2 86 16 16 MVA HN1 H 3.333 0.000 1 87 17 17 ARG H H 8.422 0.001 1 88 17 17 ARG HA H 4.590 0.001 1 89 17 17 ARG HB2 H 1.836 0.002 2 90 17 17 ARG HB3 H 1.729 0.003 2 91 17 17 ARG HG2 H 1.616 0.001 2 92 17 17 ARG HG3 H 1.539 0.001 2 93 17 17 ARG HD2 H 3.141 0.001 1 94 17 17 ARG HD3 H 3.141 0.001 1 95 17 17 ARG HE H 7.197 0.000 1 96 18 18 CYS H H 8.922 0.000 1 97 18 18 CYS HA H 5.005 0.000 1 98 18 18 CYS HB2 H 3.408 0.000 2 99 18 18 CYS HB3 H 3.047 0.000 2 100 19 19 ASP H H 8.669 0.001 1 101 19 19 ASP HA H 5.140 0.002 1 102 19 19 ASP HB2 H 2.732 0.002 2 103 19 19 ASP HB3 H 2.542 0.002 2 104 20 20 DPR HA H 4.739 0.001 1 105 20 20 DPR HB2 H 2.316 0.002 2 106 20 20 DPR HB3 H 1.937 0.002 2 107 20 20 DPR HD2 H 3.865 0.002 2 108 20 20 DPR HD3 H 3.530 0.000 2 109 20 20 DPR HG2 H 2.172 0.002 2 110 20 20 DPR HG3 H 2.027 0.001 2 111 21 21 PRO HA H 4.544 0.000 1 112 21 21 PRO HB2 H 2.256 0.002 2 113 21 21 PRO HB3 H 2.121 0.000 2 114 21 21 PRO HG2 H 2.104 0.003 2 115 21 21 PRO HG3 H 1.902 0.002 2 116 21 21 PRO HD2 H 4.008 0.001 2 117 21 21 PRO HD3 H 3.732 0.002 2 118 22 22 ARG H H 7.641 0.000 1 119 22 22 ARG HA H 4.478 0.001 1 120 22 22 ARG HB2 H 1.848 0.002 1 121 22 22 ARG HB3 H 1.848 0.002 1 122 22 22 ARG HG2 H 1.574 0.001 1 123 22 22 ARG HG3 H 1.574 0.001 1 124 22 22 ARG HD2 H 3.206 0.002 1 125 22 22 ARG HD3 H 3.206 0.002 1 126 22 22 ARG HE H 7.215 0.000 1 127 23 23 TYR H H 8.103 0.000 1 128 23 23 TYR HA H 5.284 0.001 1 129 23 23 TYR HB2 H 2.793 0.000 2 130 23 23 TYR HB3 H 2.694 0.000 2 131 23 23 TYR HD1 H 6.759 0.000 1 132 23 23 TYR HD2 H 6.759 0.000 1 133 23 23 TYR HE1 H 6.726 0.000 1 134 23 23 TYR HE2 H 6.726 0.000 1 135 24 24 GLU H H 8.876 0.001 1 136 24 24 GLU HA H 5.108 0.001 1 137 24 24 GLU HB2 H 1.949 0.001 2 138 24 24 GLU HB3 H 1.868 0.002 2 139 24 24 GLU HG2 H 2.322 0.002 1 140 24 24 GLU HG3 H 2.322 0.002 1 141 25 25 MVA HA H 4.919 0.001 1 142 25 25 MVA HB H 2.066 0.001 1 143 25 25 MVA HG11 H 0.340 0.001 2 144 25 25 MVA HG21 H 0.588 0.001 2 145 25 25 MVA HN1 H 3.172 0.000 1 146 26 26 HIS H H 8.905 0.000 1 147 26 26 HIS HA H 5.071 0.001 1 148 26 26 HIS HB2 H 3.316 0.003 2 149 26 26 HIS HB3 H 3.137 0.001 2 150 26 26 HIS HD2 H 7.173 0.000 4 151 26 26 HIS HE1 H 8.625 0.000 4 152 27 27 CYS H H 9.203 0.002 1 153 27 27 CYS HA H 4.843 0.004 1 154 27 27 CYS HB2 H 2.902 0.000 2 155 27 27 CYS HB3 H 3.251 0.000 2 156 28 28 NH2 HN1 H 7.192 0.000 2 157 28 28 NH2 HN2 H 7.803 0.000 2 stop_ save_