data_30145 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR Solution Structure of Designed Peptide NC_cHHH_D1 ; _BMRB_accession_number 30145 _BMRB_flat_file_name bmr30145.str _Entry_type original _Submission_date 2016-07-19 _Accession_date 2016-07-19 _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 Harvey P. J. . 2 Craik D. J. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 136 "13C chemical shifts" 60 "15N chemical shifts" 22 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-02-22 update BMRB 'update entry citation' 2016-09-16 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 30138 'Designed Peptide NC_HEE_D1' 30140 'Designed Peptide NC_EHE_D1' 30141 'Designed Peptide NC_EEH_D2' 30142 'Designed Peptide NC_EEH_D1' 30143 'Designed Peptide NC_cHH_D1' 30144 'Designed Peptide NC_cHh_DL_D1' 30146 'Designed Peptide NC_cEE_D1' stop_ _Original_release_date 2016-09-16 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; Accurate de novo design of hyperstable constrained peptides. ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 27626386 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Bhardwaj G. . . 2 Mulligan V. K. . 3 Bahl C. D. . 4 Gilmore J. M. . 5 Harvey P. J. . 6 Cheneval O. . . 7 Buchko G. W. . 8 Pulavarti S. V. . 9 Kaas Q. . . 10 Eletsky A. . . 11 Huang P. S. . 12 Johnsen W. A. . 13 Greisen P. J. . 14 Rocklin G. J. . 15 Song Y. . . 16 Linsky T. W. . 17 Watkins A. . . 18 Rettie S. A. . 19 Xu X. . . 20 Carter L. P. . 21 Bonneau R. . . 22 Olson J. M. . 23 Coutsias E. . . 24 Correnti C. E. . 25 Szyperski T. . . 26 Craik D. J. . 27 Baker D. . . stop_ _Journal_abbreviation Nature _Journal_volume 538 _Journal_issue 7625 _Journal_ASTM NATUAS _Journal_ISSN 1476-4687 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 329 _Page_last 335 _Year 2016 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Designed peptide NC_cHHH_D1' _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 2563.837 _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 22 _Mol_residue_sequence ; NPEDCRQDPEANKSPEECKK LK ; loop_ _Residue_seq_code _Residue_label 1 ASN 2 PRO 3 GLU 4 ASP 5 CYS 6 ARG 7 GLN 8 ASP 9 PRO 10 GLU 11 ALA 12 ASN 13 LYS 14 SER 15 PRO 16 GLU 17 GLU 18 CYS 19 LYS 20 LYS 21 LEU 22 LYS 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 $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 '1.0 mg/mL design peptide NC_cHHH_D1, 90% H2O/10% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1.0 mg/mL 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details '1.0 mg/mL design peptide NC_cHHH_D1, 100% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 1.0 mg/mL 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name CNS _Version . loop_ _Vendor _Address _Electronic_address 'Brunger, Adams, Clore, Gros, Nilges and Read' . . stop_ loop_ _Task refinement stop_ _Details . save_ save_software_2 _Saveframe_category software _Name CYANA _Version . loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task 'structure calculation' stop_ _Details . save_ save_software_3 _Saveframe_category software _Name CcpNMR _Version . loop_ _Vendor _Address _Electronic_address CCPN . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_software_4 _Saveframe_category software _Name TOPSPIN _Version 2.1 loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task processing stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _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_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_2 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_2 save_ save_2D_ECOSY_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D ECOSY' _Sample_label $sample_2 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 3.0 0.1 pH pressure 1 . atm temperature 283 .1 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 0.000 internal indirect . . . 0.25144953 DSS H 1 'methyl protons' ppm 0.000 internal direct . . . 1.0 DSS N 15 'methyl protons' ppm 0.000 internal indirect . . . 0.10132912 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 1H-1H TOCSY' '2D 1H-1H NOESY' '2D 1H-15N HSQC' '2D 1H-13C HSQC' '2D ECOSY' stop_ loop_ _Sample_label $sample_1 $sample_2 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 H H 8.128 0.002 1 2 1 1 ASN HA H 5.075 0.009 1 3 1 1 ASN HB2 H 2.716 0.009 2 4 1 1 ASN HB3 H 2.944 0.006 2 5 1 1 ASN HD21 H 7.719 0.002 1 6 1 1 ASN HD22 H 7.001 0.002 1 7 1 1 ASN CA C 50.717 0.000 1 8 1 1 ASN CB C 38.957 0.024 1 9 1 1 ASN N N 114.976 0.000 1 10 1 1 ASN ND2 N 112.847 0.013 1 11 2 2 PRO HA H 4.390 0.007 1 12 2 2 PRO HB2 H 1.976 0.011 2 13 2 2 PRO HB3 H 2.356 0.005 2 14 2 2 PRO HG2 H 2.068 0.002 1 15 2 2 PRO HG3 H 2.068 0.002 1 16 2 2 PRO HD2 H 3.802 0.004 1 17 2 2 PRO HD3 H 3.802 0.004 1 18 2 2 PRO CA C 64.799 0.000 1 19 2 2 PRO CB C 32.230 0.051 1 20 2 2 PRO CG C 27.598 0.000 1 21 2 2 PRO CD C 51.189 0.000 1 22 3 3 GLU H H 8.444 0.001 1 23 3 3 GLU HA H 4.160 0.007 1 24 3 3 GLU HB2 H 2.058 0.008 1 25 3 3 GLU HB3 H 2.058 0.008 1 26 3 3 GLU HG2 H 2.461 0.008 1 27 3 3 GLU HG3 H 2.461 0.008 1 28 3 3 GLU CA C 57.981 0.017 1 29 3 3 GLU CB C 28.404 0.000 1 30 3 3 GLU CG C 33.909 0.048 1 31 3 3 GLU N N 117.540 0.000 1 32 4 4 ASP H H 8.234 0.005 1 33 4 4 ASP HA H 4.609 0.012 1 34 4 4 ASP HB2 H 2.851 0.014 2 35 4 4 ASP HB3 H 2.904 0.024 2 36 4 4 ASP CA C 54.866 0.112 1 37 4 4 ASP CB C 39.056 0.161 1 38 4 4 ASP N N 118.778 0.000 1 39 5 5 CYS H H 7.792 0.004 1 40 5 5 CYS HA H 4.296 0.010 1 41 5 5 CYS HB2 H 3.221 0.003 1 42 5 5 CYS HB3 H 3.221 0.005 1 43 5 5 CYS CA C 56.734 0.088 1 44 5 5 CYS CB C 40.390 0.004 1 45 5 5 CYS N N 118.132 0.000 1 46 6 6 ARG H H 8.068 0.004 1 47 6 6 ARG HA H 4.211 0.005 1 48 6 6 ARG HB2 H 1.851 0.004 2 49 6 6 ARG HB3 H 1.884 0.011 2 50 6 6 ARG HG2 H 1.657 0.012 2 51 6 6 ARG HG3 H 1.669 0.008 2 52 6 6 ARG HD2 H 3.222 0.002 1 53 6 6 ARG HD3 H 3.222 0.002 1 54 6 6 ARG HE H 7.356 0.001 1 55 6 6 ARG CA C 57.478 0.025 1 56 6 6 ARG CB C 30.427 0.078 1 57 6 6 ARG CG C 27.389 0.086 1 58 6 6 ARG CD C 43.327 0.051 1 59 6 6 ARG N N 119.393 0.000 1 60 7 7 GLN H H 7.948 0.005 1 61 7 7 GLN HA H 4.312 0.007 1 62 7 7 GLN HB2 H 2.010 0.009 2 63 7 7 GLN HB3 H 2.173 0.009 2 64 7 7 GLN HG2 H 2.389 0.005 2 65 7 7 GLN HG3 H 2.392 0.006 2 66 7 7 GLN HE21 H 7.574 0.002 1 67 7 7 GLN HE22 H 6.908 0.004 1 68 7 7 GLN CA C 57.553 0.000 1 69 7 7 GLN CB C 29.317 0.037 1 70 7 7 GLN CG C 33.931 0.086 1 71 7 7 GLN N N 117.544 0.000 1 72 7 7 GLN NE2 N 111.988 0.001 1 73 8 8 ASP H H 7.929 0.005 1 74 8 8 ASP HA H 5.032 0.010 1 75 8 8 ASP HB2 H 2.753 0.018 2 76 8 8 ASP HB3 H 2.978 0.014 2 77 8 8 ASP CA C 51.185 0.000 1 78 8 8 ASP CB C 39.940 0.185 1 79 8 8 ASP N N 120.043 0.000 1 80 9 9 PRO HA H 4.399 0.003 1 81 9 9 PRO HB2 H 2.362 0.003 1 82 9 9 PRO HB3 H 2.362 0.003 1 83 9 9 PRO HG2 H 2.063 0.000 1 84 9 9 PRO HG3 H 2.063 0.000 1 85 9 9 PRO HD2 H 3.862 0.003 1 86 9 9 PRO HD3 H 3.862 0.003 1 87 9 9 PRO CA C 64.814 0.000 1 88 9 9 PRO CB C 32.317 0.000 1 89 9 9 PRO CG C 27.552 0.000 1 90 9 9 PRO CD C 50.998 0.000 1 91 10 10 GLU H H 8.290 0.004 1 92 10 10 GLU HA H 4.303 0.006 1 93 10 10 GLU HB2 H 2.033 0.009 2 94 10 10 GLU HB3 H 2.164 0.010 2 95 10 10 GLU HG2 H 2.467 0.014 1 96 10 10 GLU HG3 H 2.467 0.014 1 97 10 10 GLU CA C 56.022 0.105 1 98 10 10 GLU CB C 28.504 0.028 1 99 10 10 GLU CG C 33.772 0.088 1 100 10 10 GLU N N 116.806 0.000 1 101 11 11 ALA H H 7.913 0.003 1 102 11 11 ALA HA H 4.229 0.008 1 103 11 11 ALA HB H 1.441 0.002 1 104 11 11 ALA CA C 53.253 0.010 1 105 11 11 ALA CB C 19.227 0.060 1 106 11 11 ALA N N 122.566 0.000 1 107 12 12 ASN H H 8.266 0.003 1 108 12 12 ASN HA H 4.546 0.006 1 109 12 12 ASN HB2 H 2.836 0.003 1 110 12 12 ASN HB3 H 2.836 0.003 1 111 12 12 ASN HD21 H 7.604 0.004 1 112 12 12 ASN HD22 H 6.916 0.001 1 113 12 12 ASN CA C 53.905 0.072 1 114 12 12 ASN CB C 38.506 0.080 1 115 12 12 ASN N N 115.516 0.000 1 116 12 12 ASN ND2 N 112.353 0.011 1 117 13 13 LYS H H 7.978 0.004 1 118 13 13 LYS HA H 4.383 0.005 1 119 13 13 LYS HB2 H 1.796 0.005 2 120 13 13 LYS HB3 H 1.853 0.010 2 121 13 13 LYS HG2 H 1.433 0.008 2 122 13 13 LYS HG3 H 1.428 0.009 2 123 13 13 LYS HD2 H 1.665 0.000 1 124 13 13 LYS HD3 H 1.661 0.003 1 125 13 13 LYS CA C 56.342 0.030 1 126 13 13 LYS CB C 33.425 0.059 1 127 13 13 LYS CG C 25.122 0.119 1 128 13 13 LYS N N 118.865 0.000 1 129 14 14 SER H H 8.189 0.001 1 130 14 14 SER HA H 4.861 0.004 1 131 14 14 SER HB2 H 3.927 0.004 2 132 14 14 SER HB3 H 4.052 0.007 2 133 14 14 SER CA C 55.939 0.000 1 134 14 14 SER CB C 63.404 0.032 1 135 14 14 SER N N 116.555 0.000 1 136 15 15 PRO HA H 4.359 0.006 1 137 15 15 PRO HB2 H 2.359 0.001 1 138 15 15 PRO HB3 H 2.359 0.001 1 139 15 15 PRO HG2 H 2.005 0.000 2 140 15 15 PRO HG3 H 2.134 0.000 2 141 15 15 PRO HD2 H 3.863 0.002 1 142 15 15 PRO HD3 H 3.863 0.002 1 143 15 15 PRO CA C 65.154 0.000 1 144 15 15 PRO CB C 32.312 0.000 1 145 15 15 PRO CD C 51.014 0.000 1 146 16 16 GLU H H 8.536 0.002 1 147 16 16 GLU HA H 4.107 0.007 1 148 16 16 GLU HB2 H 2.045 0.004 1 149 16 16 GLU HB3 H 2.045 0.004 1 150 16 16 GLU HG2 H 2.429 0.008 1 151 16 16 GLU HG3 H 2.429 0.008 1 152 16 16 GLU CA C 58.288 0.167 1 153 16 16 GLU CG C 34.458 0.000 1 154 16 16 GLU N N 117.610 0.000 1 155 17 17 GLU H H 8.025 0.004 1 156 17 17 GLU HA H 4.133 0.004 1 157 17 17 GLU HB2 H 2.167 0.008 1 158 17 17 GLU HB3 H 2.167 0.008 1 159 17 17 GLU HG2 H 2.443 0.004 1 160 17 17 GLU HG3 H 2.443 0.004 1 161 17 17 GLU CA C 58.345 0.000 1 162 17 17 GLU CB C 28.559 0.000 1 163 17 17 GLU CG C 33.861 0.000 1 164 17 17 GLU N N 119.360 0.000 1 165 18 18 CYS H H 8.391 0.004 1 166 18 18 CYS HA H 4.414 0.007 1 167 18 18 CYS HB2 H 3.224 0.001 1 168 18 18 CYS HB3 H 3.224 0.001 1 169 18 18 CYS CA C 57.780 0.027 1 170 18 18 CYS CB C 39.258 0.000 1 171 18 18 CYS N N 118.081 0.000 1 172 19 19 LYS H H 7.848 0.003 1 173 19 19 LYS HA H 4.116 0.003 1 174 19 19 LYS HB2 H 1.878 0.006 2 175 19 19 LYS HB3 H 1.887 0.013 2 176 19 19 LYS HG2 H 1.480 0.007 2 177 19 19 LYS HG3 H 1.559 0.003 2 178 19 19 LYS HD2 H 1.694 0.006 1 179 19 19 LYS HD3 H 1.694 0.006 1 180 19 19 LYS HE2 H 2.969 0.000 1 181 19 19 LYS HE3 H 2.969 0.000 1 182 19 19 LYS CA C 58.182 0.000 1 183 19 19 LYS CB C 32.682 0.005 1 184 19 19 LYS N N 117.662 0.000 1 185 20 20 LYS H H 7.508 0.006 1 186 20 20 LYS HA H 4.248 0.002 1 187 20 20 LYS HB2 H 1.818 0.000 2 188 20 20 LYS HB3 H 1.981 0.005 2 189 20 20 LYS HG2 H 1.439 0.000 1 190 20 20 LYS HG3 H 1.439 0.000 1 191 20 20 LYS HE2 H 2.975 0.000 1 192 20 20 LYS HE3 H 2.975 0.000 1 193 20 20 LYS CA C 56.976 0.000 1 194 20 20 LYS CB C 32.945 0.000 1 195 20 20 LYS N N 116.620 0.000 1 196 21 21 LEU H H 7.514 0.003 1 197 21 21 LEU HA H 4.327 0.002 1 198 21 21 LEU HB2 H 1.574 0.007 2 199 21 21 LEU HB3 H 1.740 0.007 2 200 21 21 LEU HG H 1.812 0.006 1 201 21 21 LEU HD1 H 0.966 0.004 1 202 21 21 LEU HD2 H 0.873 0.003 1 203 21 21 LEU CA C 54.873 0.088 1 204 21 21 LEU CB C 42.473 0.067 1 205 21 21 LEU CG C 27.182 0.000 1 206 21 21 LEU CD1 C 26.157 0.076 1 207 21 21 LEU CD2 C 22.614 0.088 1 208 21 21 LEU N N 119.567 0.000 1 209 22 22 LYS H H 8.388 0.004 1 210 22 22 LYS HA H 4.110 0.005 1 211 22 22 LYS HB2 H 1.840 0.005 2 212 22 22 LYS HB3 H 1.842 0.004 2 213 22 22 LYS HG2 H 1.452 0.002 1 214 22 22 LYS HG3 H 1.452 0.002 1 215 22 22 LYS CA C 58.099 0.006 1 216 22 22 LYS CB C 32.292 0.041 1 217 22 22 LYS CG C 25.025 0.000 1 218 22 22 LYS N N 119.740 0.000 1 stop_ save_