data_26913 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Partially-Deuterated Samples of HET-s(218-289) Fibrils: Assignment and Deuterium Isotope Effect ; _BMRB_accession_number 26913 _BMRB_flat_file_name bmr26913.str _Entry_type original _Submission_date 2016-09-30 _Accession_date 2016-09-30 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'HET-s backbone assignments and deuterium isotope effect investigation' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Smith Albert A. . 2 Ravotti Francesco . . 3 Testori Emilie . . 4 Cadalbert Riccardo A. . 5 Ernst Matthias . . 6 Boeckmann Anja . . 7 Meier Beat H. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 3 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 155 "13C chemical shifts" 230 "15N chemical shifts" 86 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-05-23 update BMRB 'update entry citation' 2017-01-30 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 11028 'rigid core of the HET-s(218-289) prion protein in its amyloid conformation' 11064 'rigid core of the HET-s(218-289) prion protein in its amyloid conformation' stop_ _Original_release_date 2016-09-30 save_ ############################# # Citation for this entry # ############################# save_Smith_HETs_assign _Saveframe_category entry_citation _Citation_full . _Citation_title ; Partially-deuterated samples of HET-s(218-289) fibrils: assignment and deuterium isotope effect ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 28074361 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Smith Albert A. . 2 Ravotti Francesco . . 3 Testori Emilie . . 4 Cadalbert Riccardo A. . 5 Ernst Matthias . . 6 Boeckmann Anja . . 7 Meier Beat H. . stop_ _Journal_abbreviation 'J. Biomol. NMR' _Journal_volume 67 _Journal_issue 2 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 109 _Page_last 119 _Year 2017 _Details . loop_ _Keyword 'assignment strategy' 'deuterium isotope effect' fibrils 'magic-angle spinning' 'solid-state NMR' stop_ save_ ####################################### # Cited references within the entry # ####################################### save_Siemer_HET-s _Saveframe_category citation _Citation_full . _Citation_title ; 13C, 15N Resonance assignment of parts of the HET-s prion protein in its amyloid form ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 16518695 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Siemer Ansgar B. . 2 Ritter Christiane . . 3 Steinmetz Michel O. . 4 Ernst Matthias . . 5 Riek Roland . . 6 Meier Beat H. . stop_ _Journal_abbreviation 'J. Biomol. NMR' _Journal_name_full . _Journal_volume 34 _Journal_issue 2 _Journal_CSD . _Book_title . _Book_chapter_title . _Book_volume . _Book_series . _Book_publisher . _Book_publisher_city . _Book_ISBN . _Conference_title . _Conference_site . _Conference_state_province . _Conference_country . _Conference_start_date . _Conference_end_date . _Conference_abstract_number . _Thesis_institution . _Thesis_institution_city . _Thesis_institution_country . _Page_first 75 _Page_last 87 _Year 2006 _Details . save_ save_van_Melckebeke_HETs _Saveframe_category citation _Citation_full . _Citation_title ; Atomic-Resolution Three-Dimensional Structure of HET-s(218-289) Amyloid Fibrils by Solid-State NMR Spectroscopy ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 20828131 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 'Van Melckebeke' Helene . . 2 Wasmer Christian . . 3 Lange Adam . . 4 AB Eiso . . 5 Loquet Antoine . . 6 Boeckmann Anja . . 7 Meier Beat H. . stop_ _Journal_abbreviation 'J. Am. Chem. Soc.' _Journal_name_full . _Journal_volume 132 _Journal_issue 39 _Journal_CSD . _Book_title . _Book_chapter_title . _Book_volume . _Book_series . _Book_publisher . _Book_publisher_city . _Book_ISBN . _Conference_title . _Conference_site . _Conference_state_province . _Conference_country . _Conference_start_date . _Conference_end_date . _Conference_abstract_number . _Thesis_institution . _Thesis_institution_city . _Thesis_institution_country . _Page_first 13765 _Page_last 13775 _Year 2010 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name HET-s(218-289) _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'HET-s(218-289) fibrils' $HET-s_(218-289) stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . loop_ _Biological_function 'amyloid fibrils' 'heterokaryon incompatibility' 'prion protein' stop_ _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_HET-s_(218-289) _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common HET-s_(218-289) _Molecular_mass 8667.732 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 79 _Mol_residue_sequence ; MKIDAIVGRNSAKDIRTEER ARVQLGNVVTAAALHGGIRI SDQTTNSVETVVGKGESRVL IGNEYGGKGFWDNHHHHHH ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 217 MET 2 218 LYS 3 219 ILE 4 220 ASP 5 221 ALA 6 222 ILE 7 223 VAL 8 224 GLY 9 225 ARG 10 226 ASN 11 227 SER 12 228 ALA 13 229 LYS 14 230 ASP 15 231 ILE 16 232 ARG 17 233 THR 18 234 GLU 19 235 GLU 20 236 ARG 21 237 ALA 22 238 ARG 23 239 VAL 24 240 GLN 25 241 LEU 26 242 GLY 27 243 ASN 28 244 VAL 29 245 VAL 30 246 THR 31 247 ALA 32 248 ALA 33 249 ALA 34 250 LEU 35 251 HIS 36 252 GLY 37 253 GLY 38 254 ILE 39 255 ARG 40 256 ILE 41 257 SER 42 258 ASP 43 259 GLN 44 260 THR 45 261 THR 46 262 ASN 47 263 SER 48 264 VAL 49 265 GLU 50 266 THR 51 267 VAL 52 268 VAL 53 269 GLY 54 270 LYS 55 271 GLY 56 272 GLU 57 273 SER 58 274 ARG 59 275 VAL 60 276 LEU 61 277 ILE 62 278 GLY 63 279 ASN 64 280 GLU 65 281 TYR 66 282 GLY 67 283 GLY 68 284 LYS 69 285 GLY 70 286 PHE 71 287 TRP 72 288 ASP 73 289 ASN 74 290 HIS 75 291 HIS 76 292 HIS 77 293 HIS 78 294 HIS 79 295 HIS 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 $HET-s_(218-289) 'Podospora anserina' 5145 Eukaryota Fungi Podospora anserina 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 $HET-s_(218-289) 'recombinant technology' . Escherichia coli . pET-24a stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_HN_sample _Saveframe_category sample _Sample_type solid _Details ; Uniformly 13C, 15N, 2H labelled HET-s (218-289), fibrillized in H2O for 100% back exchange of 1H at exchangeable sites. ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $HET-s_(218-289) . '% w/w' 25 40 '100%-HN [U-13C; U-15N; U-2H]' H2O . '% w/w' 60 75 'natural abundance' stop_ save_ save_HA_sample _Saveframe_category sample _Sample_type solid _Details ; Uniformly 13C,15N HET-s(218-289) grown in uniformly 2H,13C labelled glucose and 25%/75% D2O/H2O for 25% protonation at the HA positions, and reduced protation elsewhere. Fibrillized in 100% D2O for no protonation at exchangeable sites. ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $HET-s_(218-289) . '% w/w' 25 40 '100% DN [U-100% 13C; U-100% 15N, 75%-D]' D2O . '% w/w' 60 75 [U-2H] stop_ save_ save_HA_HN_sample _Saveframe_category sample _Sample_type solid _Details ; Uniformly 13C,15N HET-s(218-289) grown in uniformly 2H,13C labelled glucose and 25%/75% D2O/H2O for 25% protonation at the HA positions, and reduced protation elsewhere. Fibrillized in 100% H2O for full protonation at exchangeable sites. ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $HET-s_(218-289) . '% w/w' 25 40 '100% DN [U-100% 13C; U-100% 15N, 75%-D]' H2O . '% w/w' 60 75 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CCPNMR _Saveframe_category software _Name CCPNMR _Version 2.2 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 processing stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 850 _Details . save_ ############################# # NMR applied experiments # ############################# save_3D_HACACB_1 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HACACB' _Sample_label $HA_sample save_ save_3D_NCAHA_2 _Saveframe_category NMR_applied_experiment _Experiment_name '3D NCAHA' _Sample_label $HA_HN_sample save_ save_2D_HACA_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D HACA' _Sample_label $HA_sample save_ save_3D_HNCA_4 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCA' _Sample_label $HN_sample save_ save_2D_HN_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D HN' _Sample_label $HN_sample 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' 0 . M pH 5.0 . pH pressure 1 . atm temperature 296.3 0.3 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_HA-CA-CB_shifts _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $CCPNMR $TOPSPIN stop_ loop_ _Experiment_label '3D HACACB' '2D HACA' stop_ loop_ _Sample_label $HA_sample stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'HET-s(218-289) fibrils' _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 1 223 7 VAL HA H 4.430 0.020 . 2 223 7 VAL CA C 58.762 0.100 . 3 223 7 VAL CB C 31.730 0.100 . 4 224 8 GLY HA2 H 4.644 0.020 . 5 224 8 GLY CA C 43.483 0.100 . 6 225 9 ARG HA H 5.386 0.039 . 7 225 9 ARG CA C 54.366 0.100 . 8 225 9 ARG CB C 32.557 0.100 . 9 226 10 ASN HA H 5.978 0.020 . 10 226 10 ASN CA C 51.893 0.100 . 11 226 10 ASN CB C 39.578 0.100 . 12 227 11 SER HA H 5.949 0.020 . 13 227 11 SER HB2 H 3.816 0.020 . 14 227 11 SER CA C 56.472 0.100 . 15 227 11 SER CB C 66.369 0.100 . 16 228 12 ALA HA H 5.905 0.020 . 17 228 12 ALA CA C 49.223 0.100 . 18 228 12 ALA CB C 22.983 0.100 . 19 229 13 LYS HA H 4.722 0.020 . 20 229 13 LYS CA C 59.539 0.100 . 21 229 13 LYS CB C 31.625 0.100 . 22 230 14 ASP HA H 5.793 0.020 . 23 230 14 ASP CA C 52.963 0.100 . 24 230 14 ASP CB C 44.555 0.100 . 25 231 15 ILE HA H 4.769 0.020 . 26 231 15 ILE CA C 60.723 0.100 . 27 231 15 ILE CB C 40.835 0.100 . 28 232 16 ARG HA H 5.675 0.020 . 29 232 16 ARG CA C 53.990 0.100 . 30 232 16 ARG CB C 32.046 0.100 . 31 233 17 THR HA H 5.438 0.020 . 32 233 17 THR CA C 59.400 0.100 . 33 233 17 THR CB C 71.434 0.100 . 34 234 18 GLU HA H 4.558 0.020 . 35 234 18 GLU CA C 53.561 0.100 . 36 234 18 GLU CB C 33.057 0.100 . 37 235 19 GLU HA H 3.922 0.020 . 38 235 19 GLU CA C 58.523 0.100 . 39 235 19 GLU CB C 26.630 0.100 . 40 236 20 ARG HA H 4.513 0.020 . 41 236 20 ARG CA C 54.487 0.100 . 42 236 20 ARG CB C 29.736 0.100 . 43 237 21 ALA HA H 4.351 0.020 . 44 237 21 ALA HB H 1.146 0.020 . 45 237 21 ALA CA C 52.893 0.100 . 46 237 21 ALA CB C 19.043 0.100 . 47 238 22 ARG HA H 5.941 0.020 . 48 238 22 ARG CA C 54.310 0.100 . 49 238 22 ARG CB C 34.943 0.100 . 50 239 23 VAL HA H 5.583 0.022 . 51 239 23 VAL CA C 59.771 0.100 . 52 239 23 VAL CB C 35.976 0.100 . 53 240 24 GLN HA H 5.569 0.020 . 54 240 24 GLN CA C 52.437 0.100 . 55 240 24 GLN CB C 32.092 0.100 . 56 241 25 LEU HA H 5.226 0.020 . 57 241 25 LEU CA C 52.515 0.100 . 58 241 25 LEU CB C 43.797 0.100 . 59 242 26 GLY HA2 H 3.950 0.020 . 60 242 26 GLY HA3 H 4.488 0.020 . 61 242 26 GLY CA C 43.471 0.100 . 62 243 27 ASN HA H 5.510 0.020 . 63 243 27 ASN CA C 50.977 0.100 . 64 243 27 ASN CB C 39.567 0.100 . 65 244 28 VAL HA H 4.560 0.020 . 66 244 28 VAL CA C 61.747 0.100 . 67 244 28 VAL CB C 33.516 0.100 . 68 245 29 VAL HA H 4.700 0.020 . 69 245 29 VAL CA C 61.012 0.100 . 70 245 29 VAL CB C 30.999 0.100 . 71 246 30 THR HA H 4.475 0.020 . 72 246 30 THR CA C 62.130 0.100 . 73 246 30 THR CB C 70.401 0.100 . 74 247 31 ALA HA H 3.934 0.020 . 75 247 31 ALA HB H 1.357 0.020 . 76 247 31 ALA CA C 55.874 0.100 . 77 247 31 ALA CB C 16.266 0.100 . 78 248 32 ALA HA H 4.147 0.020 . 79 248 32 ALA CA C 54.683 0.100 . 80 248 32 ALA CB C 17.606 0.100 . 81 249 33 ALA HA H 4.203 0.020 . 82 249 33 ALA CA C 53.564 0.100 . 83 260 44 THR HA H 4.318 0.020 . 84 260 44 THR CA C 65.892 0.100 . 85 261 45 THR HA H 5.367 0.020 . 86 261 45 THR CA C 61.044 0.100 . 87 261 45 THR CB C 70.175 0.100 . 88 262 46 ASN HA H 6.072 0.020 . 89 262 46 ASN CA C 52.158 0.100 . 90 262 46 ASN CB C 40.285 0.100 . 91 263 47 SER HA H 5.671 0.020 . 92 263 47 SER HB2 H 3.660 0.020 . 93 263 47 SER CA C 56.100 0.100 . 94 263 47 SER CB C 65.482 0.100 . 95 264 48 VAL HA H 6.069 0.020 . 96 264 48 VAL CA C 56.932 0.100 . 97 264 48 VAL CB C 34.806 0.100 . 98 265 49 GLU HA H 4.803 0.020 . 99 265 49 GLU CA C 59.268 0.100 . 100 265 49 GLU CB C 28.752 0.100 . 101 266 50 THR HA H 5.605 0.020 . 102 266 50 THR CA C 60.730 0.100 . 103 266 50 THR CB C 71.190 0.100 . 104 267 51 VAL HA H 5.072 0.020 . 105 267 51 VAL CA C 60.419 0.100 . 106 267 51 VAL CB C 34.754 0.100 . 107 268 52 VAL HA H 5.319 0.023 . 108 268 52 VAL CA C 61.003 0.100 . 109 268 52 VAL CB C 33.411 0.100 . 110 269 53 GLY HA2 H 3.025 0.020 . 111 269 53 GLY HA3 H 5.088 0.020 . 112 269 53 GLY CA C 44.207 0.100 . 113 270 54 LYS HA H 4.904 0.020 . 114 270 54 LYS CA C 54.101 0.100 . 115 270 54 LYS CB C 34.434 0.100 . 116 271 55 GLY HA2 H 3.900 0.020 . 117 271 55 GLY CA C 48.098 0.100 . 118 272 56 GLU HA H 4.420 0.020 . 119 272 56 GLU CA C 53.878 0.100 . 120 272 56 GLU CB C 29.235 0.100 . 121 273 57 SER HA H 4.341 0.020 . 122 273 57 SER HB2 H 4.126 0.020 . 123 273 57 SER CA C 59.033 0.100 . 124 273 57 SER CB C 65.950 0.100 . 125 274 58 ARG HA H 6.063 0.030 . 126 274 58 ARG CA C 54.694 0.100 . 127 274 58 ARG CB C 34.632 0.100 . 128 275 59 VAL HA H 5.460 0.020 . 129 275 59 VAL CA C 60.146 0.142 . 130 275 59 VAL CB C 35.374 0.100 . 131 276 60 LEU HA H 5.024 0.020 . 132 276 60 LEU CA C 52.412 0.100 . 133 276 60 LEU CB C 42.661 0.100 . 134 277 61 ILE HA H 4.862 0.020 . 135 277 61 ILE CA C 58.599 0.100 . 136 277 61 ILE CB C 34.945 0.100 . 137 278 62 GLY HA2 H 3.652 0.020 . 138 278 62 GLY HA3 H 4.913 0.020 . 139 278 62 GLY CA C 43.640 0.100 . 140 279 63 ASN HA H 5.012 0.020 . 141 279 63 ASN CA C 51.585 0.100 . 142 279 63 ASN CB C 40.041 0.100 . 143 280 64 GLU HA H 5.139 0.020 . 144 280 64 GLU CA C 54.395 0.100 . 145 280 64 GLU CB C 32.522 0.100 . 146 281 65 TYR HA H 5.559 0.020 . 147 281 65 TYR CA C 55.892 0.100 . 148 281 65 TYR CB C 39.605 0.100 . 149 282 66 GLY HA2 H 3.226 0.020 . 150 282 66 GLY HA3 H 4.557 0.023 . 151 282 66 GLY CA C 45.783 0.168 . 152 283 67 GLY HA2 H 3.791 0.020 . 153 283 67 GLY CA C 43.839 0.100 . 154 284 68 LYS HA H 5.661 0.020 . 155 284 68 LYS CA C 57.081 0.100 . 156 284 68 LYS CB C 34.634 0.100 . 157 286 70 PHE HA H 3.463 0.020 . 158 286 70 PHE CA C 59.367 0.100 . 159 286 70 PHE CB C 40.553 0.100 . 160 287 71 TRP HA H 4.140 0.020 . 161 287 71 TRP CA C 56.787 0.100 . stop_ save_ save_HN_shifts _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $CCPNMR $TOPSPIN stop_ loop_ _Experiment_label '3D HNCA' '2D HN' stop_ loop_ _Sample_label $HN_sample stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'HET-s(218-289) fibrils' _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 1 225 9 ARG C C 173.998 0.100 . 2 226 10 ASN H H 9.043 0.020 . 3 226 10 ASN C C 174.556 0.100 . 4 226 10 ASN CA C 51.748 0.100 . 5 226 10 ASN N N 124.599 0.100 . 6 227 11 SER H H 9.426 0.020 . 7 227 11 SER C C 171.921 0.100 . 8 227 11 SER CA C 56.343 0.100 . 9 227 11 SER N N 118.181 0.100 . 10 228 12 ALA H H 8.621 0.020 . 11 228 12 ALA C C 176.854 0.100 . 12 228 12 ALA CA C 49.126 0.100 . 13 228 12 ALA N N 121.854 0.100 . 14 229 13 LYS H H 8.183 0.020 . 15 229 13 LYS C C 175.216 0.100 . 16 229 13 LYS CA C 59.364 0.100 . 17 229 13 LYS N N 122.802 0.100 . 18 230 14 ASP H H 8.519 0.020 . 19 230 14 ASP C C 174.518 0.100 . 20 230 14 ASP CA C 52.707 0.100 . 21 230 14 ASP N N 116.818 0.100 . 22 231 15 ILE H H 8.768 0.020 . 23 231 15 ILE C C 174.547 0.100 . 24 231 15 ILE CA C 60.543 0.100 . 25 231 15 ILE N N 122.027 0.101 . 26 232 16 ARG H H 9.093 0.020 . 27 232 16 ARG CA C 53.836 0.100 . 28 232 16 ARG N N 128.972 0.100 . 29 233 17 THR H H 8.698 0.020 . 30 233 17 THR C C 174.421 0.100 . 31 233 17 THR CA C 59.189 0.100 . 32 233 17 THR N N 112.650 0.100 . 33 234 18 GLU H H 8.267 0.020 . 34 234 18 GLU C C 173.822 0.100 . 35 234 18 GLU CA C 53.389 0.100 . 36 234 18 GLU N N 118.865 0.100 . 37 235 19 GLU H H 9.284 0.020 . 38 235 19 GLU C C 174.128 0.100 . 39 235 19 GLU CA C 58.370 0.100 . 40 235 19 GLU N N 116.240 0.100 . 41 236 20 ARG H H 8.740 0.020 . 42 236 20 ARG C C 176.382 0.100 . 43 236 20 ARG CA C 54.275 0.100 . 44 236 20 ARG N N 122.188 0.100 . 45 237 21 ALA H H 7.790 0.020 . 46 237 21 ALA C C 176.000 0.100 . 47 237 21 ALA CA C 52.731 0.100 . 48 237 21 ALA N N 125.080 0.100 . 49 238 22 ARG H H 8.300 0.020 . 50 238 22 ARG C C 175.502 0.100 . 51 238 22 ARG CA C 54.096 0.100 . 52 238 22 ARG N N 117.421 0.100 . 53 239 23 VAL H H 8.583 0.020 . 54 239 23 VAL C C 173.186 0.100 . 55 239 23 VAL CA C 59.610 0.100 . 56 239 23 VAL N N 121.804 0.100 . 57 240 24 GLN H H 9.123 0.020 . 58 240 24 GLN C C 173.091 0.100 . 59 240 24 GLN CA C 52.337 0.100 . 60 240 24 GLN N N 125.736 0.100 . 61 241 25 LEU H H 9.125 0.020 . 62 241 25 LEU C C 172.813 0.100 . 63 241 25 LEU CA C 52.404 0.100 . 64 241 25 LEU N N 130.568 0.100 . 65 242 26 GLY H H 8.848 0.020 . 66 242 26 GLY C C 170.656 0.100 . 67 242 26 GLY CA C 43.319 0.100 . 68 242 26 GLY N N 112.810 0.100 . 69 243 27 ASN H H 8.390 0.020 . 70 243 27 ASN C C 176.282 0.100 . 71 243 27 ASN CA C 50.875 0.100 . 72 243 27 ASN N N 109.218 0.111 . 73 244 28 VAL H H 9.143 0.020 . 74 244 28 VAL C C 174.370 0.100 . 75 244 28 VAL CA C 61.563 0.100 . 76 244 28 VAL N N 122.085 0.100 . 77 245 29 VAL H H 9.023 0.020 . 78 245 29 VAL C C 175.360 0.100 . 79 245 29 VAL CA C 60.753 0.100 . 80 245 29 VAL N N 128.382 0.100 . 81 246 30 THR H H 8.315 0.020 . 82 246 30 THR C C 175.286 0.100 . 83 246 30 THR CA C 62.034 0.100 . 84 246 30 THR N N 115.606 0.100 . 85 247 31 ALA H H 8.730 0.020 . 86 247 31 ALA C C 179.740 0.100 . 87 247 31 ALA CA C 55.519 0.100 . 88 247 31 ALA N N 119.928 0.100 . 89 248 32 ALA H H 8.343 0.020 . 90 248 32 ALA CA C 54.580 0.100 . 91 248 32 ALA N N 118.913 0.100 . 92 249 33 ALA H H 7.720 0.043 . 93 249 33 ALA CA C 53.591 0.100 . 94 249 33 ALA N N 119.429 0.100 . 95 260 44 THR C C 175.186 0.100 . 96 261 45 THR H H 8.371 0.020 . 97 261 45 THR C C 172.289 0.100 . 98 261 45 THR CA C 60.932 0.100 . 99 261 45 THR N N 123.295 0.100 . 100 262 46 ASN H H 8.959 0.020 . 101 262 46 ASN C C 174.443 0.100 . 102 262 46 ASN CA C 52.119 0.100 . 103 262 46 ASN N N 126.783 0.100 . 104 263 47 SER H H 8.729 0.020 . 105 263 47 SER C C 171.568 0.100 . 106 263 47 SER CA C 55.979 0.100 . 107 263 47 SER N N 116.623 0.100 . 108 264 48 VAL H H 8.713 0.020 . 109 264 48 VAL C C 174.476 0.100 . 110 264 48 VAL CA C 56.720 0.100 . 111 264 48 VAL N N 124.406 0.100 . 112 265 49 GLU H H 7.868 0.020 . 113 265 49 GLU C C 175.818 0.100 . 114 265 49 GLU CA C 58.976 0.100 . 115 265 49 GLU N N 126.403 0.100 . 116 266 50 THR H H 8.855 0.020 . 117 266 50 THR C C 172.900 0.100 . 118 266 50 THR CA C 60.655 0.100 . 119 266 50 THR N N 112.412 0.126 . 120 267 51 VAL H H 8.663 0.020 . 121 267 51 VAL C C 175.021 0.100 . 122 267 51 VAL CA C 60.200 0.100 . 123 267 51 VAL N N 123.710 0.100 . 124 268 52 VAL H H 8.792 0.020 . 125 268 52 VAL C C 175.090 0.100 . 126 268 52 VAL CA C 60.769 0.100 . 127 268 52 VAL N N 127.487 0.100 . 128 269 53 GLY H H 8.673 0.020 . 129 269 53 GLY C C 171.988 0.100 . 130 269 53 GLY CA C 44.087 0.100 . 131 269 53 GLY N N 112.492 0.100 . 132 270 54 LYS H H 8.136 0.020 . 133 270 54 LYS C C 176.877 0.100 . 134 270 54 LYS CA C 53.893 0.100 . 135 270 54 LYS N N 120.812 0.100 . 136 271 55 GLY H H 9.753 0.020 . 137 271 55 GLY C C 172.125 0.100 . 138 271 55 GLY CA C 47.990 0.100 . 139 271 55 GLY N N 114.434 0.100 . 140 272 56 GLU H H 9.219 0.020 . 141 272 56 GLU C C 176.413 0.100 . 142 272 56 GLU CA C 53.733 0.100 . 143 272 56 GLU N N 127.757 0.100 . 144 273 57 SER H H 7.587 0.020 . 145 273 57 SER C C 173.389 0.100 . 146 273 57 SER CA C 58.864 0.100 . 147 273 57 SER N N 115.605 0.100 . 148 274 58 ARG H H 8.655 0.020 . 149 274 58 ARG CA C 54.597 0.100 . 150 274 58 ARG N N 117.288 0.100 . 151 275 59 VAL H H 8.879 0.020 . 152 275 59 VAL C C 172.694 0.100 . 153 275 59 VAL CA C 59.993 0.100 . 154 275 59 VAL N N 121.961 0.100 . 155 276 60 LEU H H 8.401 0.020 . 156 276 60 LEU C C 173.767 0.100 . 157 276 60 LEU CA C 52.254 0.100 . 158 276 60 LEU N N 129.532 0.100 . 159 277 61 ILE H H 9.389 0.020 . 160 277 61 ILE C C 173.405 0.100 . 161 277 61 ILE CA C 58.414 0.100 . 162 277 61 ILE N N 129.341 0.100 . 163 278 62 GLY H H 8.468 0.020 . 164 278 62 GLY C C 171.991 0.100 . 165 278 62 GLY CA C 43.543 0.100 . 166 278 62 GLY N N 110.474 0.100 . 167 279 63 ASN H H 8.530 0.026 . 168 279 63 ASN C C 172.914 0.100 . 169 279 63 ASN CA C 51.357 0.100 . 170 279 63 ASN N N 113.839 0.100 . 171 280 64 GLU H H 8.799 0.020 . 172 280 64 GLU C C 174.745 0.100 . 173 280 64 GLU CA C 54.177 0.100 . 174 280 64 GLU N N 119.741 0.100 . 175 281 65 TYR H H 9.871 0.031 . 176 281 65 TYR C C 176.188 0.100 . 177 281 65 TYR CA C 55.731 0.100 . 178 281 65 TYR N N 128.151 0.100 . 179 282 66 GLY H H 9.751 0.035 . 180 282 66 GLY C C 172.751 0.100 . 181 282 66 GLY CA C 45.563 0.100 . 182 282 66 GLY N N 108.909 0.120 . 183 283 67 GLY H H 8.369 0.020 . 184 283 67 GLY CA C 43.359 0.100 . 185 283 67 GLY N N 111.849 0.100 . 186 284 68 LYS C C 177.766 0.100 . 187 285 69 GLY H H 9.120 0.020 . 188 285 69 GLY CA C 43.900 0.100 . 189 285 69 GLY N N 107.786 0.132 . stop_ save_ save_HA-CA-N_shifts _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $CCPNMR $TOPSPIN stop_ loop_ _Experiment_label '3D NCAHA' stop_ loop_ _Sample_label $HA_HN_sample stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name 'HET-s(218-289) fibrils' _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 1 228 12 ALA HA H 5.908 0.020 . 2 228 12 ALA CA C 49.168 0.100 . 3 228 12 ALA N N 121.872 0.100 . 4 229 13 LYS HA H 4.680 0.020 . 5 229 13 LYS CA C 59.708 0.100 . 6 229 13 LYS N N 122.640 0.100 . 7 230 14 ASP HA H 5.785 0.020 . 8 230 14 ASP CA C 52.973 0.100 . 9 230 14 ASP N N 116.629 0.100 . 10 231 15 ILE HA H 4.765 0.020 . 11 231 15 ILE CA C 60.733 0.100 . 12 231 15 ILE N N 121.793 0.100 . 13 232 16 ARG HA H 5.684 0.020 . 14 232 16 ARG CA C 53.985 0.100 . 15 232 16 ARG N N 128.759 0.100 . 16 233 17 THR H H 8.768 0.020 . 17 233 17 THR HA H 5.451 0.020 . 18 233 17 THR CA C 59.260 0.108 . 19 233 17 THR N N 112.409 0.104 . 20 234 18 GLU HA H 4.560 0.020 . 21 234 18 GLU CA C 53.443 0.100 . 22 234 18 GLU N N 118.870 0.100 . 23 235 19 GLU HA H 3.927 0.020 . 24 235 19 GLU CA C 58.384 0.100 . 25 235 19 GLU N N 116.064 0.100 . 26 236 20 ARG HA H 4.539 0.020 . 27 236 20 ARG CA C 54.461 0.100 . 28 236 20 ARG N N 122.056 0.100 . 29 237 21 ALA HA H 4.367 0.020 . 30 237 21 ALA CA C 52.970 0.100 . 31 237 21 ALA N N 125.051 0.100 . 32 238 22 ARG HA H 5.973 0.020 . 33 238 22 ARG CA C 54.206 0.100 . 34 238 22 ARG N N 117.406 0.100 . 35 239 23 VAL HA H 5.578 0.020 . 36 239 23 VAL CA C 59.980 0.100 . 37 239 23 VAL N N 122.099 0.100 . 38 240 24 GLN H H 9.165 0.020 . 39 240 24 GLN HA H 5.595 0.020 . 40 240 24 GLN CA C 52.347 0.139 . 41 240 24 GLN N N 125.546 0.105 . 42 242 26 GLY HA2 H 3.938 0.020 . 43 242 26 GLY HA3 H 4.435 0.020 . 44 242 26 GLY CA C 43.479 0.100 . 45 242 26 GLY N N 112.210 0.100 . 46 243 27 ASN HA H 5.610 0.020 . 47 243 27 ASN CA C 51.115 0.100 . 48 244 28 VAL HA H 4.546 0.020 . 49 244 28 VAL CA C 61.977 0.100 . 50 244 28 VAL N N 122.331 0.100 . 51 245 29 VAL HA H 4.691 0.020 . 52 245 29 VAL CA C 60.878 0.100 . 53 245 29 VAL N N 128.009 0.100 . 54 246 30 THR HA H 4.500 0.020 . 55 246 30 THR CA C 62.012 0.100 . 56 246 30 THR N N 115.792 0.100 . 57 247 31 ALA HA H 3.933 0.020 . 58 247 31 ALA CA C 55.998 0.100 . 59 247 31 ALA N N 119.802 0.100 . 60 248 32 ALA HA H 4.197 0.020 . 61 248 32 ALA CA C 54.820 0.100 . 62 248 32 ALA N N 118.303 0.100 . 63 264 48 VAL HA H 6.073 0.020 . 64 264 48 VAL CA C 56.828 0.100 . 65 264 48 VAL N N 124.508 0.100 . 66 265 49 GLU HA H 4.810 0.020 . 67 265 49 GLU CA C 59.250 0.100 . 68 265 49 GLU N N 126.291 0.100 . 69 266 50 THR HA H 5.630 0.020 . 70 266 50 THR CA C 60.800 0.100 . 71 266 50 THR N N 111.858 0.100 . 72 267 51 VAL HA H 5.070 0.020 . 73 267 51 VAL CA C 60.483 0.100 . 74 267 51 VAL N N 123.395 0.100 . 75 268 52 VAL HA H 5.312 0.020 . 76 268 52 VAL CA C 61.029 0.100 . 77 268 52 VAL N N 127.334 0.100 . 78 269 53 GLY HA2 H 3.022 0.020 . 79 269 53 GLY HA3 H 5.095 0.020 . 80 269 53 GLY CA C 44.134 0.100 . 81 269 53 GLY N N 112.408 0.100 . 82 270 54 LYS HA H 4.924 0.020 . 83 270 54 LYS CA C 54.078 0.100 . 84 270 54 LYS N N 120.787 0.100 . 85 271 55 GLY HA2 H 3.913 0.020 . 86 271 55 GLY CA C 47.988 0.100 . 87 271 55 GLY N N 114.216 0.100 . 88 272 56 GLU HA H 4.417 0.020 . 89 272 56 GLU CA C 53.910 0.100 . 90 272 56 GLU N N 127.617 0.100 . 91 273 57 SER H H 7.666 0.020 . 92 273 57 SER HA H 4.334 0.020 . 93 273 57 SER CA C 59.064 0.109 . 94 273 57 SER N N 115.477 0.100 . 95 274 58 ARG HA H 6.089 0.020 . 96 274 58 ARG CA C 54.766 0.100 . 97 274 58 ARG N N 117.355 0.100 . 98 275 59 VAL HA H 5.410 0.020 . 99 275 59 VAL CA C 59.980 0.100 . 100 275 59 VAL N N 122.099 0.100 . 101 276 60 LEU HA H 5.045 0.020 . 102 276 60 LEU CA C 52.418 0.100 . 103 276 60 LEU N N 129.329 0.100 . 104 277 61 ILE HA H 4.777 0.020 . 105 277 61 ILE CA C 58.617 0.100 . 106 277 61 ILE N N 129.244 0.100 . 107 278 62 GLY HA2 H 3.697 0.020 . 108 278 62 GLY CA C 43.361 0.100 . 109 278 62 GLY N N 110.613 0.100 . 110 280 64 GLU HA H 5.168 0.020 . 111 280 64 GLU CA C 54.557 0.100 . 112 280 64 GLU N N 119.728 0.100 . 113 281 65 TYR HA H 5.559 0.020 . 114 281 65 TYR CA C 56.177 0.100 . 115 281 65 TYR N N 128.402 0.100 . 116 283 67 GLY HA2 H 3.770 0.020 . 117 283 67 GLY CA C 43.806 0.100 . 118 283 67 GLY N N 112.956 0.100 . 119 287 71 TRP HA H 4.100 0.020 . 120 287 71 TRP CA C 56.750 0.100 . 121 287 71 TRP N N 117.614 0.100 . stop_ save_