data_27065 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 13C, 15N chemical shift assignments of MAK33 VL S20N amyloid fibrils ; _BMRB_accession_number 27065 _BMRB_flat_file_name bmr27065.str _Entry_type original _Submission_date 2017-04-06 _Accession_date 2017-04-06 _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 Hora Manuel . . 2 Sarkar Riddhiman . . 3 Morris Vanessa . . 4 Xue Kai . . 5 Prade Elke . . 6 Harding Emma . . 7 Buchner Johannes . . 8 Reif Bernd . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "13C chemical shifts" 111 "15N chemical shifts" 34 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-08-11 update BMRB 'update entry citation' 2017-04-27 original author 'original release' stop_ _Original_release_date 2017-04-06 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; MAK33 antibody light chain amyloid fibrils are similar to oligomeric precursors. ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 28746363 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Hora Manuel . . 2 Sarkar Riddhiman . . 3 Morris Vanessa . . 4 Xue Kai . . 5 Prade Elke . . 6 Harding Emma . . 7 Buchner Johannes . . 8 Reif Bernd . . stop_ _Journal_abbreviation 'PLoS ONE' _Journal_name_full 'PloS one' _Journal_volume 12 _Journal_issue 7 _Journal_ISSN 1932-6203 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first e0181799 _Page_last e0181799 _Year 2017 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'MAK33 VL amyloid fibril' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'MAK33 VL amyloid fibril' $MAK33_VL stop_ _System_molecular_weight . _System_physical_state 'amyloid fibril' _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_MAK33_VL _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common MAK33_VL _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 108 _Mol_residue_sequence ; DIVLTQSPATLSVTPGDSVN LSCRASQSISNNLHWYQQKS HESPRLLIKYASQSISGIPS RFSGSGSGTDFTLSINSVET EDFGMYFCQQSNSWPLTFGA GTKLELKR ; loop_ _Residue_seq_code _Residue_label 1 ASP 2 ILE 3 VAL 4 LEU 5 THR 6 GLN 7 SER 8 PRO 9 ALA 10 THR 11 LEU 12 SER 13 VAL 14 THR 15 PRO 16 GLY 17 ASP 18 SER 19 VAL 20 ASN 21 LEU 22 SER 23 CYS 24 ARG 25 ALA 26 SER 27 GLN 28 SER 29 ILE 30 SER 31 ASN 32 ASN 33 LEU 34 HIS 35 TRP 36 TYR 37 GLN 38 GLN 39 LYS 40 SER 41 HIS 42 GLU 43 SER 44 PRO 45 ARG 46 LEU 47 LEU 48 ILE 49 LYS 50 TYR 51 ALA 52 SER 53 GLN 54 SER 55 ILE 56 SER 57 GLY 58 ILE 59 PRO 60 SER 61 ARG 62 PHE 63 SER 64 GLY 65 SER 66 GLY 67 SER 68 GLY 69 THR 70 ASP 71 PHE 72 THR 73 LEU 74 SER 75 ILE 76 ASN 77 SER 78 VAL 79 GLU 80 THR 81 GLU 82 ASP 83 PHE 84 GLY 85 MET 86 TYR 87 PHE 88 CYS 89 GLN 90 GLN 91 SER 92 ASN 93 SER 94 TRP 95 PRO 96 LEU 97 THR 98 PHE 99 GLY 100 ALA 101 GLY 102 THR 103 LYS 104 LEU 105 GLU 106 LEU 107 LYS 108 ARG 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 $MAK33_VL Mouse 10090 Eukaryota Metazoa Mus musculus stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Variant _Vector_name $MAK33_VL 'recombinant technology' . Escherichia coli K12 'BL 21' 'pET 28a' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solid _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $MAK33_VL . mM '[U-13C; U-15N]' 'acetic acid' 25 mM 'natural abundance' 'phosphoric acid' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'sodium azide' 0.05 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CcpNMR_Analysis _Saveframe_category software _Name CcpNMR_Analysis _Version 2 loop_ _Vendor _Address _Electronic_address CCPN . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 750 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_PDSD_(50_ms)_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D PDSD (50 ms)' _Sample_label $sample_1 save_ save_2D_NCACX_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D NCACX' _Sample_label $sample_1 save_ save_3D_NCACX_3 _Saveframe_category NMR_applied_experiment _Experiment_name '3D NCACX' _Sample_label $sample_1 save_ save_2D_NCOCX_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D NCOCX' _Sample_label $sample_1 save_ save_3D_NCOCX_5 _Saveframe_category NMR_applied_experiment _Experiment_name '3D NCOCX' _Sample_label $sample_1 save_ save_2D_NCACB_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D NCACB' _Sample_label $sample_1 save_ save_3D_NCACB_7 _Saveframe_category NMR_applied_experiment _Experiment_name '3D NCACB' _Sample_label $sample_1 save_ save_2D_NcoCACB_8 _Saveframe_category NMR_applied_experiment _Experiment_name '2D NcoCACB' _Sample_label $sample_1 save_ save_3D_NCOCA_9 _Saveframe_category NMR_applied_experiment _Experiment_name '3D NCOCA' _Sample_label $sample_1 save_ save_3D_CANCO_10 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CANCO' _Sample_label $sample_1 save_ save_2D_15N_INEPT_11 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 15N INEPT' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details '273 K was set temperature; MAS heated the sample above 273 K' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 175 . mM pH 2 . 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 MLF C 13 'methyl carbon' ppm 54.4 external direct . . . 1 MLF N 15 nitrogen ppm 116.2 external direct . . . 1 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_ _Experiment_label '2D PDSD (50 ms)' '2D NCACX' '3D NCACX' '2D NCOCX' '3D NCOCX' '2D NCACB' '3D NCACB' '2D NcoCACB' '3D NCOCA' '3D CANCO' 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 'MAK33 VL amyloid fibril' _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 49 49 LYS C C 173.792 0.089 1 2 49 49 LYS CA C 52.898 0.000 1 3 50 50 TYR C C 171.732 0.054 1 4 50 50 TYR CA C 54.675 0.152 1 5 50 50 TYR CB C 39.580 0.148 1 6 50 50 TYR N N 121.513 0.091 1 7 51 51 ALA C C 171.479 0.065 1 8 51 51 ALA CA C 50.158 0.068 1 9 51 51 ALA CB C 19.174 0.009 1 10 51 51 ALA N N 130.104 0.130 1 11 52 52 SER C C 171.283 0.000 1 12 52 52 SER CA C 55.455 0.042 1 13 52 52 SER CB C 64.986 0.038 1 14 52 52 SER N N 112.198 0.140 1 15 60 60 SER C C 171.004 0.181 1 16 60 60 SER CA C 55.262 0.084 1 17 60 60 SER CB C 65.052 0.123 1 18 60 60 SER N N 112.531 0.119 1 19 61 61 ARG C C 173.726 0.055 1 20 61 61 ARG CA C 52.940 0.102 1 21 61 61 ARG CB C 32.135 0.122 1 22 61 61 ARG CG C 26.039 0.173 1 23 61 61 ARG CD C 41.645 0.053 1 24 61 61 ARG N N 118.300 0.267 1 25 62 62 PHE C C 170.738 0.121 1 26 62 62 PHE CA C 59.559 0.098 1 27 62 62 PHE CB C 42.841 0.000 1 28 62 62 PHE N N 118.779 0.033 1 29 63 63 SER C C 172.554 0.088 1 30 63 63 SER CA C 54.577 0.090 1 31 63 63 SER CB C 63.037 0.056 1 32 63 63 SER N N 121.495 0.123 1 33 64 64 GLY C C 172.688 0.129 1 34 64 64 GLY CA C 46.221 0.086 1 35 64 64 GLY N N 111.353 0.074 1 36 65 65 SER C C 176.008 0.051 1 37 65 65 SER CA C 55.470 0.095 1 38 65 65 SER CB C 61.727 0.058 1 39 65 65 SER N N 106.308 0.118 1 40 66 66 GLY C C 171.508 0.074 1 41 66 66 GLY CA C 44.710 0.093 1 42 66 66 GLY N N 104.123 0.174 1 43 67 67 SER C C 171.639 0.088 1 44 67 67 SER CA C 56.773 0.131 1 45 67 67 SER CB C 63.262 0.026 1 46 67 67 SER N N 114.671 0.173 1 47 68 68 GLY C C 171.931 0.002 1 48 68 68 GLY CA C 43.645 0.150 1 49 68 68 GLY N N 108.687 0.068 1 50 69 69 THR C C 171.542 0.189 1 51 69 69 THR CA C 61.203 0.086 1 52 69 69 THR CB C 69.792 0.091 1 53 69 69 THR CG2 C 21.054 0.096 1 54 69 69 THR N N 122.092 0.181 1 55 70 70 ASP C C 171.720 0.095 1 56 70 70 ASP CA C 50.551 0.137 1 57 70 70 ASP CB C 38.737 0.082 1 58 70 70 ASP CG C 175.221 0.000 1 59 70 70 ASP N N 125.025 0.124 1 60 71 71 PHE C C 171.899 0.150 1 61 71 71 PHE CA C 50.782 0.096 1 62 71 71 PHE CB C 39.178 0.000 1 63 71 71 PHE N N 122.610 0.001 1 64 72 72 THR C C 171.780 0.031 1 65 72 72 THR CA C 61.340 0.080 1 66 72 72 THR CB C 69.260 0.000 1 67 72 72 THR CG2 C 21.341 0.000 1 68 72 72 THR N N 122.591 0.043 1 69 73 73 LEU C C 173.264 0.149 1 70 73 73 LEU CA C 52.322 0.059 1 71 73 73 LEU CB C 44.038 0.131 1 72 73 73 LEU CG C 26.832 0.082 1 73 73 73 LEU CD1 C 24.033 0.182 1 74 73 73 LEU N N 125.002 0.216 1 75 74 74 SER C C 174.795 0.083 1 76 74 74 SER CA C 54.543 0.069 1 77 74 74 SER CB C 60.753 0.060 1 78 74 74 SER N N 115.577 0.161 1 79 75 75 ILE C C 173.363 0.038 1 80 75 75 ILE CA C 61.679 0.138 1 81 75 75 ILE CB C 41.866 0.100 1 82 75 75 ILE CG1 C 27.175 0.150 1 83 75 75 ILE CG2 C 16.723 0.095 1 84 75 75 ILE CD1 C 13.467 0.054 1 85 75 75 ILE N N 127.399 0.137 1 86 76 76 ASN C C 171.422 0.123 1 87 76 76 ASN CA C 52.037 0.043 1 88 76 76 ASN CB C 39.315 0.098 1 89 76 76 ASN N N 132.745 0.219 1 90 77 77 SER C C 172.713 0.075 1 91 77 77 SER CA C 54.030 0.087 1 92 77 77 SER CB C 65.292 0.096 1 93 77 77 SER N N 115.037 0.073 1 94 78 78 VAL C C 173.408 0.075 1 95 78 78 VAL CA C 66.244 0.105 1 96 78 78 VAL CB C 27.474 0.097 1 97 78 78 VAL CG1 C 22.421 0.065 2 98 78 78 VAL CG2 C 20.657 0.072 2 99 78 78 VAL N N 119.544 0.247 1 100 79 79 GLU C C 172.202 0.051 1 101 79 79 GLU CA C 52.499 0.108 1 102 79 79 GLU CB C 31.692 0.146 1 103 79 79 GLU CG C 34.871 0.032 1 104 79 79 GLU CD C 179.915 0.095 1 105 79 79 GLU N N 118.950 0.117 1 106 80 80 THR C C 172.111 0.131 1 107 80 80 THR CA C 60.112 0.198 1 108 80 80 THR CB C 72.004 0.033 1 109 80 80 THR CG2 C 19.662 0.158 1 110 80 80 THR N N 122.477 0.173 1 111 81 81 GLU N N 121.908 0.000 1 112 82 82 ASP C C 170.568 0.009 1 113 82 82 ASP CA C 51.313 0.000 1 114 83 83 PHE C C 170.459 0.113 1 115 83 83 PHE CA C 51.761 0.059 1 116 83 83 PHE CB C 38.405 0.061 1 117 83 83 PHE N N 111.913 0.208 1 118 84 84 GLY C C 170.232 0.128 1 119 84 84 GLY CA C 41.603 0.073 1 120 84 84 GLY N N 102.055 0.079 1 121 85 85 MET C C 173.708 0.114 1 122 85 85 MET CA C 51.756 0.159 1 123 85 85 MET CB C 34.593 0.056 1 124 85 85 MET N N 116.523 0.174 1 125 86 86 TYR C C 174.172 0.057 1 126 86 86 TYR CA C 52.593 0.062 1 127 86 86 TYR CB C 32.303 0.036 1 128 86 86 TYR N N 115.836 0.090 1 129 87 87 PHE C C 171.592 0.039 1 130 87 87 PHE CA C 54.856 0.164 1 131 87 87 PHE CB C 39.177 0.050 1 132 87 87 PHE N N 121.987 0.071 1 133 98 98 PHE C C 175.848 0.025 1 134 98 98 PHE CA C 54.818 0.034 1 135 98 98 PHE CB C 41.488 0.000 1 136 98 98 PHE N N 113.385 0.023 1 137 99 99 GLY C C 170.578 0.048 1 138 99 99 GLY CA C 42.655 0.033 1 139 99 99 GLY N N 107.434 0.063 1 140 100 100 ALA C C 177.202 0.078 1 141 100 100 ALA CA C 51.591 0.038 1 142 100 100 ALA CB C 17.163 0.037 1 143 100 100 ALA N N 120.706 0.066 1 144 101 101 GLY CA C 44.867 0.000 1 145 101 101 GLY N N 105.670 0.083 1 stop_ save_