data_27420 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Chemical shifts for the de novo mini protein gHH_44 in the reduced state. ; _BMRB_accession_number 27420 _BMRB_flat_file_name bmr27420.str _Entry_type original _Submission_date 2018-03-06 _Accession_date 2018-03-06 _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 Buchko Garry W. . 2 Bahl Christopher . . 3 Baker David . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 143 "13C chemical shifts" 72 "15N chemical shifts" 28 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2018-10-26 update BMRB 'update entry citation' 2018-04-11 original author 'original release' stop_ _Original_release_date 2018-03-07 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Cytosolic expression, solution structures, and molecular dynamics simulation of genetically encodable disulfide-rich de novo designed peptides ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 30152054 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Buchko Garry W. . 2 Pulavarti Surya . . 3 Ovchinnikov Victor . . 4 Shaw Elizabeth A. . 5 Rettie Stephen A. . 6 Myler Peter J. . 7 Karplus Martin . . 8 Szyperski Thomas . . 9 Baker David . . 10 Bahl Christopher D. . stop_ _Journal_abbreviation 'Protein Sci.' _Journal_name_full 'Protein science : a publication of the Protein Society' _Journal_volume 27 _Journal_issue 9 _Journal_ISSN 1469-896X _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 1611 _Page_last 1623 _Year 2018 _Details . loop_ _Keyword cysteine-rich 'drug design' 'drug discovery' 'peptide topology' 'structural biology' stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name gHH_44 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label gHH_44 $gHH_44 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_gHH_44 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common gHH_44 _Molecular_mass . _Mol_thiol_state 'all free' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 28 _Mol_residue_sequence ; AEDCERIRKELEKNPNDEIK KKLEKCQA ; loop_ _Residue_seq_code _Residue_label 1 ALA 2 GLU 3 ASP 4 CYS 5 GLU 6 ARG 7 ILE 8 ARG 9 LYS 10 GLU 11 LEU 12 GLU 13 LYS 14 ASN 15 PRO 16 ASN 17 ASP 18 GLU 19 ILE 20 LYS 21 LYS 22 LYS 23 LEU 24 GLU 25 LYS 26 CYS 27 GLN 28 ALA 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 $gHH_44 . . . . . . 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 $gHH_44 'recombinant technology' . Escherichia coli . pCDB368 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 $gHH_44 1 mM '[U-99% 13C; U-99% 15N]' 'sodium acetate' 20 mM 'natural abundance' TCEP 5 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_Felix _Saveframe_category software _Name Felix _Version 2007 loop_ _Vendor _Address _Electronic_address 'Accelrys Software Inc.' . . stop_ loop_ _Task processing stop_ _Details . save_ save_SPARKY _Saveframe_category software _Name SPARKY _Version 1.4 loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Agilent _Model VXRS _Field_strength 800 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Agilent _Model VXRS _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_2D_1H-13C_HSQC_aliphatic_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $sample_1 save_ save_3D_C(CO)NH_3 _Saveframe_category NMR_applied_experiment _Experiment_name '3D C(CO)NH' _Sample_label $sample_1 save_ save_3D_HNCACB_4 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCACB' _Sample_label $sample_1 save_ save_3D_C(CO)NH_5 _Saveframe_category NMR_applied_experiment _Experiment_name '3D C(CO)NH' _Sample_label $sample_1 save_ save_3D_1H-15N_NOESY_6 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N NOESY' _Sample_label $sample_1 save_ save_3D_1H-13C_NOESY_aliphatic_7 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-13C NOESY aliphatic' _Sample_label $sample_1 save_ save_3D_HNCO_8 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _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' 25 . mM pH 4.8 . pH pressure 1 . atm temperature 273 . 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_ _Software_label $SPARKY stop_ loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-13C HSQC aliphatic' '3D C(CO)NH' '3D HNCACB' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name gHH_44 _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 ALA HA H 4.15 0.02 1 2 1 1 ALA HB H 1.57 0.02 1 3 1 1 ALA CA C 51.7 0.2 1 4 1 1 ALA CB C 19.4 0.2 1 5 2 2 GLU H H 8.80 0.02 1 6 2 2 GLU HA H 4.37 0.02 1 7 2 2 GLU HB2 H 2.06 0.02 2 8 2 2 GLU HB3 H 1.97 0.02 2 9 2 2 GLU HG2 H 2.33 0.02 2 10 2 2 GLU HG3 H 2.33 0.02 2 11 2 2 GLU CA C 56.1 0.2 1 12 2 2 GLU CB C 30.3 0.2 1 13 2 2 GLU CG C 35.5 0.2 1 14 2 2 GLU N N 120.5 0.2 1 15 3 3 ASP H H 8.64 0.02 1 16 3 3 ASP HA H 4.37 0.02 1 17 3 3 ASP HB2 H 2.85 0.02 2 18 3 3 ASP HB3 H 2.75 0.02 2 19 3 3 ASP CA C 56.1 0.2 1 20 3 3 ASP CB C 40.7 0.2 1 21 3 3 ASP N N 121.6 0.2 1 22 4 4 CYS H H 8.63 0.02 1 23 4 4 CYS HA H 4.45 0.02 1 24 4 4 CYS HB2 H 3.13 0.02 2 25 4 4 CYS HB3 H 3.00 0.02 2 26 4 4 CYS CA C 57.1 0.2 1 27 4 4 CYS CB C 39.2 0.2 1 28 4 4 CYS N N 120.2 0.2 1 29 5 5 GLU H H 8.45 0.02 1 30 5 5 GLU HA H 4.11 0.02 1 31 5 5 GLU HB2 H 2.14 0.02 2 32 5 5 GLU HB3 H 2.07 0.02 2 33 5 5 GLU HG2 H 2.36 0.02 2 34 5 5 GLU HG3 H 2.36 0.02 2 35 5 5 GLU CB C 28.6 0.2 1 36 5 5 GLU CG C 35.1 0.2 1 37 5 5 GLU N N 120.5 0.2 1 38 6 6 ARG H H 7.90 0.02 1 39 6 6 ARG HA H 4.04 0.02 1 40 6 6 ARG HB2 H 1.92 0.02 2 41 6 6 ARG HB3 H 1.92 0.02 2 42 6 6 ARG HG2 H 1.73 0.02 2 43 6 6 ARG HG3 H 1.62 0.02 2 44 6 6 ARG HD2 H 3.24 0.02 2 45 6 6 ARG HD3 H 3.24 0.02 2 46 6 6 ARG CA C 59.1 0.2 1 47 6 6 ARG CB C 29.8 0.2 1 48 6 6 ARG CG C 27.4 0.2 1 49 6 6 ARG CD C 43.3 0.2 1 50 6 6 ARG N N 119.4 0.2 1 51 7 7 ILE H H 7.66 0.02 1 52 7 7 ILE HA H 3.78 0.02 1 53 7 7 ILE HB H 1.91 0.02 1 54 7 7 ILE HG12 H 1.71 0.02 2 55 7 7 ILE HG13 H 1.08 0.02 2 56 7 7 ILE HG2 H 0.87 0.02 1 57 7 7 ILE HD1 H 0.83 0.02 1 58 7 7 ILE CA C 64.2 0.2 1 59 7 7 ILE CB C 37.7 0.2 1 60 7 7 ILE CG1 C 28.4 0.2 1 61 7 7 ILE CG2 C 18.6 0.2 1 62 7 7 ILE CD1 C 13.7 0.2 1 63 7 7 ILE N N 119.2 0.2 1 64 8 8 ARG H H 8.19 0.02 1 65 8 8 ARG HA H 3.86 0.02 1 66 8 8 ARG HB2 H 1.91 0.02 2 67 8 8 ARG HB3 H 1.91 0.02 2 68 8 8 ARG HG2 H 1.74 0.02 2 69 8 8 ARG HG3 H 1.58 0.02 2 70 8 8 ARG HD2 H 3.22 0.02 2 71 8 8 ARG HD3 H 3.22 0.02 2 72 8 8 ARG CA C 60.1 0.2 1 73 8 8 ARG CB C 29.9 0.2 1 74 8 8 ARG CG C 28.3 0.2 1 75 8 8 ARG CD C 43.1 0.2 1 76 8 8 ARG N N 119.9 0.2 1 77 9 9 LYS H H 7.93 0.02 1 78 9 9 LYS HA H 4.08 0.02 1 79 9 9 LYS N N 117.9 0.2 1 80 10 10 GLU H H 7.92 0.02 1 81 10 10 GLU HA H 4.09 0.02 1 82 10 10 GLU HB2 H 2.66 0.02 2 83 10 10 GLU HB3 H 2.14 0.02 2 84 10 10 GLU HG2 H 2.51 0.02 2 85 10 10 GLU HG3 H 2.35 0.02 2 86 10 10 GLU CB C 28.8 0.2 1 87 10 10 GLU CG C 35.3 0.2 1 88 10 10 GLU N N 120.3 0.2 1 89 11 11 LEU HA H 4.02 0.02 1 90 11 11 LEU HB2 H 1.87 0.02 2 91 11 11 LEU HB3 H 1.60 0.02 2 92 11 11 LEU HG H 1.68 0.02 1 93 11 11 LEU HD1 H 0.95 0.02 2 94 11 11 LEU HD2 H 0.92 0.02 2 95 11 11 LEU CA C 56.9 0.2 1 96 11 11 LEU CB C 41.8 0.2 1 97 11 11 LEU CG C 26.8 0.2 1 98 11 11 LEU CD1 C 25.4 0.2 2 99 11 11 LEU CD2 C 25.6 0.2 2 100 12 12 GLU H H 7.67 0.02 1 101 12 12 GLU HA H 3.98 0.02 1 102 12 12 GLU HB2 H 2.10 0.02 2 103 12 12 GLU HB3 H 2.10 0.02 2 104 12 12 GLU HG2 H 2.51 0.02 2 105 12 12 GLU HG3 H 2.31 0.02 2 106 12 12 GLU CA C 58.2 0.2 1 107 12 12 GLU CB C 29.4 0.2 1 108 12 12 GLU CG C 35.6 0.2 1 109 12 12 GLU N N 116.2 0.2 1 110 13 13 LYS H H 7.38 0.02 1 111 13 13 LYS HA H 4.26 0.02 1 112 13 13 LYS HB2 H 1.89 0.02 2 113 13 13 LYS HB3 H 1.84 0.02 2 114 13 13 LYS HG2 H 1.53 0.02 2 115 13 13 LYS HG3 H 1.47 0.02 2 116 13 13 LYS CA C 57.1 0.2 1 117 13 13 LYS CB C 33.3 0.2 1 118 13 13 LYS CG C 24.8 0.2 1 119 13 13 LYS N N 116.4 0.2 1 120 14 14 ASN H H 8.01 0.02 1 121 14 14 ASN HA H 5.05 0.02 1 122 14 14 ASN HB2 H 2.83 0.02 2 123 14 14 ASN HB3 H 2.67 0.02 2 124 14 14 ASN HD21 H 6.92 0.02 2 125 14 14 ASN HD22 H 7.71 0.02 2 126 14 14 ASN CA C 51.1 0.2 1 127 14 14 ASN CB C 39.3 0.2 1 128 14 14 ASN N N 115.6 0.2 1 129 14 14 ASN ND2 N 112.4 0.2 1 130 15 15 PRO HA H 4.46 0.02 1 131 15 15 PRO HB2 H 2.27 0.02 2 132 15 15 PRO HB3 H 2.01 0.02 2 133 15 15 PRO HG2 H 2.06 0.02 2 134 15 15 PRO HG3 H 2.05 0.02 2 135 15 15 PRO HD2 H 3.69 0.02 2 136 15 15 PRO HD3 H 3.49 0.02 2 137 15 15 PRO CA C 63.7 0.2 1 138 15 15 PRO CB C 31.1 0.2 1 139 15 15 PRO CG C 27.3 0.2 1 140 15 15 PRO CD C 49.9 0.2 1 141 16 16 ASN H H 8.64 0.02 1 142 16 16 ASN HA H 4.72 0.02 1 143 16 16 ASN HB2 H 2.98 0.02 2 144 16 16 ASN HB3 H 2.90 0.02 2 145 16 16 ASN HD21 H 7.61 0.02 2 146 16 16 ASN HD22 H 6.97 0.02 2 147 16 16 ASN CA C 53.0 0.2 1 148 16 16 ASN CB C 39.8 0.2 1 149 16 16 ASN N N 121.6 0.2 1 150 16 16 ASN ND2 N 113.8 0.2 1 151 17 17 ASP H H 8.72 0.02 1 152 17 17 ASP HA H 4.40 0.02 1 153 17 17 ASP HB2 H 2.68 0.02 2 154 17 17 ASP HB3 H 2.68 0.02 2 155 17 17 ASP CA C 57.1 0.2 1 156 17 17 ASP CB C 40.9 0.2 1 157 17 17 ASP N N 120.9 0.2 1 158 18 18 GLU H H 8.41 0.02 1 159 18 18 GLU HA H 4.10 0.02 1 160 18 18 GLU N N 120.6 0.2 1 161 19 19 ILE H H 8.25 0.02 1 162 19 19 ILE HA H 3.86 0.02 1 163 19 19 ILE HB H 1.94 0.02 1 164 19 19 ILE HG12 H 1.64 0.02 2 165 19 19 ILE HG13 H 1.28 0.02 2 166 19 19 ILE HG2 H 0.96 0.02 1 167 19 19 ILE HD1 H 0.89 0.02 1 168 19 19 ILE CA C 63.2 0.2 1 169 19 19 ILE CB C 37.1 0.2 1 170 19 19 ILE CG1 C 28.5 0.2 1 171 19 19 ILE CG2 C 18.7 0.2 1 172 19 19 ILE CD1 C 12.6 0.2 1 173 19 19 ILE N N 120.4 0.2 1 174 20 20 LYS H H 7.94 0.02 1 175 20 20 LYS HA H 3.90 0.02 1 176 20 20 LYS HB2 H 1.95 0.02 2 177 20 20 LYS HB3 H 1.91 0.02 2 178 20 20 LYS CA C 60.0 0.2 1 179 20 20 LYS CB C 32.5 0.2 1 180 20 20 LYS N N 121.1 0.2 1 181 21 21 LYS H H 8.87 0.02 1 182 21 21 LYS HA H 4.11 0.02 1 183 21 21 LYS CA C 58.8 0.2 1 184 21 21 LYS CB C 32.0 0.2 1 185 21 21 LYS N N 118.5 0.2 1 186 22 22 LYS H H 7.77 0.02 1 187 22 22 LYS HA H 4.06 0.02 1 188 22 22 LYS HB2 H 2.04 0.02 2 189 22 22 LYS HB3 H 1.89 0.02 2 190 22 22 LYS CB C 32.6 0.2 1 191 22 22 LYS N N 119.4 0.2 1 192 23 23 LEU H H 8.18 0.02 1 193 23 23 LEU HA H 4.08 0.02 1 194 23 23 LEU HB2 H 1.94 0.02 2 195 23 23 LEU HB3 H 1.54 0.02 2 196 23 23 LEU HG H 1.65 0.02 1 197 23 23 LEU HD1 H 0.92 0.02 2 198 23 23 LEU HD2 H 0.89 0.02 2 199 23 23 LEU CA C 57.2 0.2 1 200 23 23 LEU CB C 41.3 0.2 1 201 23 23 LEU CG C 26.7 0.2 1 202 23 23 LEU CD1 C 24.6 0.2 2 203 23 23 LEU CD2 C 25.7 0.2 2 204 23 23 LEU N N 120.5 0.2 1 205 24 24 GLU H H 7.96 0.02 1 206 24 24 GLU HA H 4.08 0.02 1 207 24 24 GLU N N 118.7 0.2 1 208 25 25 LYS H H 7.66 0.02 1 209 25 25 LYS HA H 4.32 0.02 1 210 25 25 LYS HB2 H 1.99 0.02 2 211 25 25 LYS HB3 H 1.84 0.02 2 212 25 25 LYS HG2 H 1.54 0.02 2 213 25 25 LYS HG3 H 1.47 0.02 2 214 25 25 LYS CA C 56.7 0.2 1 215 25 25 LYS CB C 32.3 0.2 1 216 25 25 LYS CG C 24.9 0.2 1 217 25 25 LYS N N 116.6 0.2 1 218 26 26 CYS H H 7.83 0.02 1 219 26 26 CYS HA H 4.50 0.02 1 220 26 26 CYS HB2 H 3.30 0.02 2 221 26 26 CYS HB3 H 3.18 0.02 2 222 26 26 CYS CA C 57.8 0.2 1 223 26 26 CYS CB C 41.6 0.2 1 224 26 26 CYS N N 118.9 0.2 1 225 27 27 GLN H H 8.26 0.02 1 226 27 27 GLN HA H 4.37 0.02 1 227 27 27 GLN HB2 H 2.17 0.02 2 228 27 27 GLN HB3 H 2.04 0.02 2 229 27 27 GLN HG2 H 2.47 0.02 2 230 27 27 GLN HG3 H 2.40 0.02 2 231 27 27 GLN HE21 H 7.56 0.02 2 232 27 27 GLN HE22 H 6.87 0.02 2 233 27 27 GLN CA C 55.9 0.2 1 234 27 27 GLN CB C 29.7 0.2 1 235 27 27 GLN CG C 34.1 0.2 1 236 27 27 GLN N N 120.4 0.2 1 237 27 27 GLN NE2 N 111.8 0.2 1 238 28 28 ALA H H 7.90 0.02 1 239 28 28 ALA HA H 4.14 0.02 1 240 28 28 ALA HB H 1.40 0.02 1 241 28 28 ALA CA C 53.9 0.2 1 242 28 28 ALA CB C 19.7 0.2 1 243 28 28 ALA N N 130.5 0.2 1 stop_ save_