data_26964 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Backbone 1H, 13C, and 15N Chemical Shift Assignments for an Exon-1 Fragment of Huntingtin at pH = 1.7 and T = 25 C. ; _BMRB_accession_number 26964 _BMRB_flat_file_name bmr26964.str _Entry_type original _Submission_date 2016-12-01 _Accession_date 2016-12-01 _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 Baias Maria . . 2 Smith Pieter E.S. . 3 Shen Koning . . 4 Joachimiak Lukasz A. . 5 Zerko Szymon . . 6 Kozminski Wiktor . . 7 Frydman Judith . . 8 Frydman Lucio . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 32 "13C chemical shifts" 96 "15N chemical shifts" 32 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-01-26 update BMRB 'update entry citation' 2016-12-29 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 26965 'Assignments at at pH = 7.1 and T = 4 C' stop_ _Original_release_date 2016-12-01 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Structure and Dynamics of the Huntingtin Exon-1 N-Terminus: A Solution NMR Perspective ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 28085263 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Baias Maria E.S. . 2 Smith Pieter E.S. . 3 Shen Koning . . 4 Joachimiak Lukasz A. . 5 Zerko Szymon . . 6 Kozminski Wiktor . . 7 Frydman Judith . . 8 Frydman Lucio . . stop_ _Journal_abbreviation 'J. Am. Chem. Soc.' _Journal_volume 139 _Journal_issue 3 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 1168 _Page_last 1176 _Year 2017 _Details . loop_ _Keyword Huntingtin 'NMR spectroscopy' 'aggregating proteins' 'intrinsically disordered peptides' 'pH conformational dependence' stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name Htt _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label Htt $Htt stop_ _System_molecular_weight . _System_physical_state 'partially disordered' _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_Htt _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common Htt _Molecular_mass . _Mol_thiol_state 'all free' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 49 _Mol_residue_sequence ; MATLEKLMKAFESLKSFQQQ QQQQQQQQQQQQQQPPPPPP LECHHHHHH ; loop_ _Residue_seq_code _Residue_label 1 MET 2 ALA 3 THR 4 LEU 5 GLU 6 LYS 7 LEU 8 MET 9 LYS 10 ALA 11 PHE 12 GLU 13 SER 14 LEU 15 LYS 16 SER 17 PHE 18 GLN 19 GLN 20 GLN 21 GLN 22 GLN 23 GLN 24 GLN 25 GLN 26 GLN 27 GLN 28 GLN 29 GLN 30 GLN 31 GLN 32 GLN 33 GLN 34 GLN 35 PRO 36 PRO 37 PRO 38 PRO 39 PRO 40 PRO 41 LEU 42 GLU 43 CYS 44 HIS 45 HIS 46 HIS 47 HIS 48 HIS 49 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 $Htt Human 9606 Eukaryota Metazoa Homo sapiens 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 $Htt 'recombinant technology' . Escherichia coli . pJexpress411 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 _Concentration_min_value _Concentration_max_value _Isotopic_labeling $Htt 125 uM 100 150 '[U-13C; U-15N]' D2O 10 % . . [U-2H] 'formic acid' 10 % . . 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_SPARKY _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Agilent _Model DD2 _Field_strength 800 _Details . save_ ############################# # NMR applied experiments # ############################# save_3D_HNCO_1 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _Sample_label $sample_1 save_ save_5D_(H)NCO(NCA)CONH_2 _Saveframe_category NMR_applied_experiment _Experiment_name '5D (H)NCO(NCA)CONH' _Sample_label $sample_1 save_ save_5D_HNCOCACB_3 _Saveframe_category NMR_applied_experiment _Experiment_name '5D HNCOCACB' _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 pH 1.66 . pH pressure 1 . atm temperature 298 . 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_ _Experiment_label '3D HNCO' '5D (H)NCO(NCA)CONH' '5D HNCOCACB' 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 Htt _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 2 2 ALA C C 173.61 0.3 1 2 2 2 ALA CA C 51.71 0.3 1 3 2 2 ALA CB C 19.34 0.3 1 4 3 3 THR H H 8.26 0.02 1 5 3 3 THR C C 173.93 0.3 1 6 3 3 THR CA C 61.61 0.3 1 7 3 3 THR CB C 69.82 0.3 1 8 3 3 THR N N 114.61 0.3 1 9 4 4 LEU H H 8.18 0.02 1 10 4 4 LEU C C 177.11 0.3 1 11 4 4 LEU CA C 55.38 0.3 1 12 4 4 LEU CB C 42.05 0.3 1 13 4 4 LEU N N 124.89 0.3 1 14 5 5 GLU H H 8.1 0.02 1 15 5 5 GLU C C 176.14 0.3 1 16 5 5 GLU CA C 56.39 0.3 1 17 5 5 GLU CB C 28.41 0.3 1 18 5 5 GLU N N 121 0.3 1 19 6 6 LYS H H 7.97 0.02 1 20 6 6 LYS C C 176.6 0.3 1 21 6 6 LYS CA C 56.92 0.3 1 22 6 6 LYS CB C 32.62 0.3 1 23 6 6 LYS N N 121.25 0.3 1 24 7 7 LEU H H 7.82 0.02 1 25 7 7 LEU C C 177.39 0.3 1 26 7 7 LEU CA C 55.38 0.3 1 27 7 7 LEU CB C 41.98 0.3 1 28 7 7 LEU N N 121.95 0.3 1 29 8 8 MET H H 7.98 0.02 1 30 8 8 MET C C 176.52 0.3 1 31 8 8 MET CA C 55.87 0.3 1 32 8 8 MET CB C 32.55 0.3 1 33 8 8 MET N N 120.45 0.3 1 34 9 9 LYS H H 7.9 0.02 1 35 9 9 LYS C C 176.65 0.3 1 36 9 9 LYS CA C 56.88 0.3 1 37 9 9 LYS CB C 32.63 0.3 1 38 9 9 LYS N N 121.23 0.3 1 39 10 10 ALA H H 7.86 0.02 1 40 10 10 ALA C C 177.85 0.3 1 41 10 10 ALA CA C 52.99 0.3 1 42 10 10 ALA CB C 18.76 0.3 1 43 10 10 ALA N N 123.47 0.3 1 44 11 11 PHE H H 7.83 0.02 1 45 11 11 PHE C C 175.99 0.3 1 46 11 11 PHE CA C 58.28 0.3 1 47 11 11 PHE CB C 39.1 0.3 1 48 11 11 PHE N N 118.43 0.3 1 49 12 12 GLU H H 7.87 0.02 1 50 12 12 GLU C C 175.98 0.3 1 51 12 12 GLU CA C 56.15 0.3 1 52 12 12 GLU CB C 28.51 0.3 1 53 12 12 GLU N N 120.19 0.3 1 54 13 13 SER H H 7.96 0.02 1 55 13 13 SER C C 174.69 0.3 1 56 13 13 SER CA C 58.55 0.3 1 57 13 13 SER CB C 63.6 0.3 1 58 13 13 SER N N 115.84 0.3 1 59 14 14 LEU H H 7.91 0.02 1 60 14 14 LEU C C 177.79 0.3 1 61 14 14 LEU CA C 56.09 0.3 1 62 14 14 LEU CB C 41.86 0.3 1 63 14 14 LEU N N 123.62 0.3 1 64 15 15 LYS H H 7.95 0.02 1 65 15 15 LYS C C 177.39 0.3 1 66 15 15 LYS CA C 57.28 0.3 1 67 15 15 LYS CB C 32.45 0.3 1 68 15 15 LYS N N 120.23 0.3 1 69 16 16 SER H H 7.89 0.02 1 70 16 16 SER C C 175.12 0.3 1 71 16 16 SER CA C 59.34 0.3 1 72 16 16 SER CB C 63.23 0.3 1 73 16 16 SER N N 115.31 0.3 1 74 17 17 PHE H H 7.94 0.02 1 75 17 17 PHE C C 176.53 0.3 1 76 17 17 PHE CA C 59.37 0.3 1 77 17 17 PHE CB C 39.01 0.3 1 78 17 17 PHE N N 122.14 0.3 1 79 18 18 GLN H H 8.08 0.02 1 80 18 18 GLN C C 177.07 0.3 1 81 18 18 GLN CA C 57.3 0.3 1 82 18 18 GLN CB C 28.62 0.3 1 83 18 18 GLN N N 119.79 0.3 1 84 19 19 GLN H H 7.96 0.02 1 85 19 19 GLN C C 177.07 0.3 1 86 19 19 GLN CA C 57.34 0.3 1 87 19 19 GLN CB C 28.67 0.3 1 88 19 19 GLN N N 119.79 0.3 1 89 20 20 GLN H H 7.97 0.02 1 90 20 20 GLN C C 177.06 0.3 1 91 20 20 GLN CA C 57.28 0.3 1 92 20 20 GLN CB C 28.61 0.3 1 93 20 20 GLN N N 120 0.3 1 94 21 21 GLN H H 7.99 0.02 1 95 21 21 GLN C C 176.98 0.3 1 96 21 21 GLN CA C 57.12 0.3 1 97 21 21 GLN CB C 28.74 0.3 1 98 21 21 GLN N N 119.72 0.3 1 99 22 22 GLN H H 7.96 0.02 1 100 22 22 GLN C C 176.89 0.3 1 101 22 22 GLN CA C 57.07 0.3 1 102 22 22 GLN CB C 28.65 0.3 1 103 22 22 GLN N N 119.81 0.3 1 104 23 23 GLN H H 7.99 0.02 1 105 23 23 GLN C C 176.81 0.3 1 106 23 23 GLN CA C 56.96 0.3 1 107 23 23 GLN CB C 28.72 0.3 1 108 23 23 GLN N N 119.91 0.3 1 109 24 24 GLN H H 8.01 0.02 1 110 24 24 GLN C C 176.75 0.3 1 111 24 24 GLN CA C 56.89 0.3 1 112 24 24 GLN CB C 28.77 0.3 1 113 24 24 GLN N N 119.96 0.3 1 114 25 25 GLN H H 8.03 0.02 1 115 25 25 GLN C C 176.68 0.3 1 116 25 25 GLN CA C 56.8 0.3 1 117 25 25 GLN CB C 28.82 0.3 1 118 25 25 GLN N N 120.02 0.3 1 119 26 26 GLN H H 8.03 0.02 1 120 26 26 GLN C C 176.6 0.3 1 121 26 26 GLN CA C 56.72 0.3 1 122 26 26 GLN CB C 28.86 0.3 1 123 26 26 GLN N N 120.06 0.3 1 124 27 27 GLN H H 8.04 0.02 1 125 27 27 GLN C C 176.51 0.3 1 126 27 27 GLN CA C 56.62 0.3 1 127 27 27 GLN CB C 28.92 0.3 1 128 27 27 GLN N N 120.09 0.3 1 129 28 28 GLN H H 8.04 0.02 1 130 28 28 GLN C C 176.4 0.3 1 131 28 28 GLN CA C 56.49 0.3 1 132 28 28 GLN CB C 28.98 0.3 1 133 28 28 GLN N N 120.14 0.3 1 134 29 29 GLN H H 8.05 0.02 1 135 29 29 GLN C C 176.32 0.3 1 136 29 29 GLN CA C 56.39 0.3 1 137 29 29 GLN CB C 29.03 0.3 1 138 29 29 GLN N N 120.2 0.3 1 139 30 30 GLN H H 8.05 0.02 1 140 30 30 GLN C C 176.14 0.3 1 141 30 30 GLN CA C 56.2 0.3 1 142 30 30 GLN CB C 29.09 0.3 1 143 30 30 GLN N N 120.26 0.3 1 144 31 31 GLN H H 8.07 0.02 1 145 31 31 GLN C C 175.91 0.3 1 146 31 31 GLN CA C 56.02 0.3 1 147 31 31 GLN CB C 29.15 0.3 1 148 31 31 GLN N N 120.44 0.3 1 149 32 32 GLN H H 8.07 0.02 1 150 32 32 GLN C C 175.69 0.3 1 151 32 32 GLN CA C 55.79 0.3 1 152 32 32 GLN CB C 29.21 0.3 1 153 32 32 GLN N N 120.58 0.3 1 154 33 33 GLN H H 8.09 0.02 1 155 33 33 GLN C C 175.42 0.3 1 156 33 33 GLN CA C 55.58 0.3 1 157 33 33 GLN CB C 29.32 0.3 1 158 33 33 GLN N N 121.03 0.3 1 159 34 34 GLN H H 8.12 0.02 1 160 34 34 GLN N N 122.33 0.3 1 stop_ save_