data_25601 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Ensemble structure the closed state of Lys63-linked diubiquitin in the absence of a ligand ; _BMRB_accession_number 25601 _BMRB_flat_file_name bmr25601.str _Entry_type original _Submission_date 2015-05-10 _Accession_date 2015-05-10 _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 Liu Zhu . . 2 Gong Zhou . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 135 "15N chemical shifts" 135 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-03-22 update BMRB 'update entry citation' 2015-07-13 original author 'original release' stop_ _Original_release_date 2015-07-13 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Lys63-linked ubiquitin chain adopts multiple conformational states for specific target recognition ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 26090905 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Liu Zhu . . 2 Gong Zhou . . 3 Yang Ju . . 4 Jiang Wen-Xue . . 5 Zhu Wen-Kai . . 6 Guo Da-Chuan . . 7 Zhang Wei-Ping . . 8 Liu Mai-Li . . 9 Tang Chun . . stop_ _Journal_abbreviation eLIFE _Journal_volume 4 _Journal_issue . _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first e05767 _Page_last e05767 _Year 2015 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'closed state of Lys63-linked diubiquitin' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label entity_1 $entity_1 entity_2 $entity_2 'S-[(1-OXYL-2,2,5,5-TETRAMETHYL-2,5-DIHYDRO-1H-PYRROL-3-YL)METHYL] METHANESULFONOTHIOATE_1' $entity_MTN 'S-[(1-OXYL-2,2,5,5-TETRAMETHYL-2,5-DIHYDRO-1H-PYRROL-3-YL)METHYL] METHANESULFONOTHIOATE_2' $entity_MTN 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_entity_1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1 _Molecular_mass 8539.906 _Mol_thiol_state . _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 76 _Mol_residue_sequence ; MQIFVKTLTGKTITLEVEPS DTIECVKAKIQDKEGIPPDQ QRLIFAGCQLEDGRTLSDYN IQKESTLHLVLRLRGG ; loop_ _Residue_seq_code _Residue_label 1 MET 2 GLN 3 ILE 4 PHE 5 VAL 6 LYS 7 THR 8 LEU 9 THR 10 GLY 11 LYS 12 THR 13 ILE 14 THR 15 LEU 16 GLU 17 VAL 18 GLU 19 PRO 20 SER 21 ASP 22 THR 23 ILE 24 GLU 25 CYS 26 VAL 27 LYS 28 ALA 29 LYS 30 ILE 31 GLN 32 ASP 33 LYS 34 GLU 35 GLY 36 ILE 37 PRO 38 PRO 39 ASP 40 GLN 41 GLN 42 ARG 43 LEU 44 ILE 45 PHE 46 ALA 47 GLY 48 CYS 49 GLN 50 LEU 51 GLU 52 ASP 53 GLY 54 ARG 55 THR 56 LEU 57 SER 58 ASP 59 TYR 60 ASN 61 ILE 62 GLN 63 LYS 64 GLU 65 SER 66 THR 67 LEU 68 HIS 69 LEU 70 VAL 71 LEU 72 ARG 73 LEU 74 ARG 75 GLY 76 GLY stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ save_entity_2 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_2 _Molecular_mass 8035.261 _Mol_thiol_state . _Details . _Residue_count 71 _Mol_residue_sequence ; MQIFVKTLTGKTITLEVEPS DTIENVKAKIQDKEGIPPDQ QRLIFAGKQLEDGRTLSDYN IQKESTLHLVL ; loop_ _Residue_seq_code _Residue_label 1 MET 2 GLN 3 ILE 4 PHE 5 VAL 6 LYS 7 THR 8 LEU 9 THR 10 GLY 11 LYS 12 THR 13 ILE 14 THR 15 LEU 16 GLU 17 VAL 18 GLU 19 PRO 20 SER 21 ASP 22 THR 23 ILE 24 GLU 25 ASN 26 VAL 27 LYS 28 ALA 29 LYS 30 ILE 31 GLN 32 ASP 33 LYS 34 GLU 35 GLY 36 ILE 37 PRO 38 PRO 39 ASP 40 GLN 41 GLN 42 ARG 43 LEU 44 ILE 45 PHE 46 ALA 47 GLY 48 LYS 49 GLN 50 LEU 51 GLU 52 ASP 53 GLY 54 ARG 55 THR 56 LEU 57 SER 58 ASP 59 TYR 60 ASN 61 ILE 62 GLN 63 LYS 64 GLU 65 SER 66 THR 67 LEU 68 HIS 69 LEU 70 VAL 71 LEU stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ############# # Ligands # ############# save_MTN _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common "entity_MTN (S-[(1-oxyl-2,2,5,5-tetramethyl-2,5-dihydro-1H-pyrrol-3-yl)methyl] methanesulfonothioate)" _BMRB_code MTN _PDB_code MTN _Molecular_mass 264.385 _Mol_charge 0 _Mol_paramagnetic . _Mol_aromatic no _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons O1 O1 O . 0 . ? N1 N1 N . 0 . ? C1 C1 C . 0 . ? C2 C2 C . 0 . ? C3 C3 C . 0 . ? C4 C4 C . 0 . ? S1 S1 S . 0 . ? C5 C5 C . 0 . ? C6 C6 C . 0 . ? C7 C7 C . 0 . ? C8 C8 C . 0 . ? C9 C9 C . 0 . ? H2 H2 H . 0 . ? H41 H41 H . 0 . ? H42 H42 H . 0 . ? H61 H61 H . 0 . ? H62 H62 H . 0 . ? H63 H63 H . 0 . ? H71 H71 H . 0 . ? H72 H72 H . 0 . ? H73 H73 H . 0 . ? H81 H81 H . 0 . ? H82 H82 H . 0 . ? H83 H83 H . 0 . ? H91 H91 H . 0 . ? H92 H92 H . 0 . ? H93 H93 H . 0 . ? S2 S2 S . 0 . ? O2 O2 O . 0 . ? O3 O3 O . 0 . ? C12 C12 C . 0 . ? H4 H4 H . 0 . ? H1 H1 H . 0 . ? H3 H3 H . 0 . ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name _PDB_bond_atom_one_atom_name _PDB_bond_atom_two_atom_name SING O1 N1 ? ? SING N1 C1 ? ? SING N1 C5 ? ? SING C1 C2 ? ? SING C1 C8 ? ? SING C1 C9 ? ? DOUB C2 C3 ? ? SING C2 H2 ? ? SING C3 C4 ? ? SING C3 C5 ? ? SING C4 S1 ? ? SING C4 H41 ? ? SING C4 H42 ? ? SING C5 C6 ? ? SING C5 C7 ? ? SING C6 H61 ? ? SING C6 H62 ? ? SING C6 H63 ? ? SING C7 H71 ? ? SING C7 H72 ? ? SING C7 H73 ? ? SING C8 H81 ? ? SING C8 H82 ? ? SING C8 H83 ? ? SING C9 H91 ? ? SING C9 H92 ? ? SING C9 H93 ? ? SING S1 S2 ? ? DOUB S2 O2 ? ? DOUB S2 O3 ? ? SING S2 C12 ? ? SING C12 H4 ? ? SING C12 H1 ? ? SING C12 H3 ? ? stop_ _Mol_thiol_state . _Sequence_homology_query_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 Human 9606 Eukaryota Metazoa Homo sapiens $entity_2 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 $entity_1 'recombinant technology' . Escherichia coli . pET11a $entity_2 'recombinant technology' . Escherichia coli . pET11a stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '0.5mM 15N_proximal-14N_distalN25C_MTS protein were prepared for the intramolecular PRE measurement.' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $assembly 0.5 mM '[U-100% 15N]' D2O 10 '% v/v' '[U-99% 2H]' 'sodium chloride' 100 mM 'natural abundance' 'sodium acetate' 10 mM 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details '0.5mM 15N_proximal-14N_distalK48C_MTS protein were prepared for the intramolecular PRE measurement.' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $assembly 0.5 mM '[U-100% 15N]' D2O 10 '% v/v' '[U-99% 2H]' 'sodium chloride' 100 mM 'natural abundance' 'sodium acetate' 10 mM 'natural abundance' stop_ save_ save_sample_3 _Saveframe_category sample _Sample_type solution _Details ; A mixture of 0.5mM 15N_proximal-14N_distal and 0.5mM 14N_proximal-14N_distalN25C_MTS protein were prepared for the intermolecular PRE measurement. ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $assembly 1 mM '[U-100% 15N]' D2O 10 '% v/v' '[U-99% 2H]' 'sodium chloride' 100 mM 'natural abundance' 'sodium acetate' 10 mM 'natural abundance' stop_ save_ save_sample_4 _Saveframe_category sample _Sample_type solution _Details ; A mixture of 0.5mM 15N_proximal-14N_distal and 0.5mM 14N_proximal-14N_distalK48C_MTS protein were prepared for the intermolecular PRE measurement. ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $assembly 1 mM '[U-100% 15N]' D2O 10 '% v/v' '[U-99% 2H]' 'sodium chloride' 100 mM 'natural abundance' 'sodium acetate' 10 mM 'natural abundance' stop_ save_ save_sample_5 _Saveframe_category sample _Sample_type solution _Details 15N_distal-14N_proximal loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $assembly 0.5 mM '[U-100% 15N]' D2O 10 '% v/v' '[U-99% 2H]' 'sodium chloride' 100 mM 'natural abundance' 'sodium acetate' 10 mM 'natural abundance' stop_ save_ save_sample_6 _Saveframe_category sample _Sample_type solution _Details 14N_distal-15N_proximal loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $assembly 0.5 mM '[U-100% 15N]' D2O 10 '% v/v' '[U-99% 2H]' 'sodium chloride' 100 mM 'natural abundance' 'sodium acetate' 10 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_X-PLOR_NIH _Saveframe_category software _Name X-PLOR_NIH _Version . loop_ _Vendor _Address _Electronic_address 'Schwieters, Kuszewski, Tjandra and Clore' . . stop_ loop_ _Task 'structure solution' stop_ _Details 'Using X-PLOR NIH to calculate the ensemble structures of Lys63-linked diubiquitin.' save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 850 _Details . save_ ############################# # NMR applied experiments # ############################# save_transverse_relaxation_rate_measurement_1 _Saveframe_category NMR_applied_experiment _Experiment_name 'transverse relaxation rate measurement' _Sample_label $sample_1 save_ save_transverse_relaxation_rate_measurement_2 _Saveframe_category NMR_applied_experiment _Experiment_name 'transverse relaxation rate measurement' _Sample_label $sample_2 save_ save_transverse_relaxation_rate_measurement_3 _Saveframe_category NMR_applied_experiment _Experiment_name 'transverse relaxation rate measurement' _Sample_label $sample_3 save_ save_transverse_relaxation_rate_measurement_4 _Saveframe_category NMR_applied_experiment _Experiment_name 'transverse relaxation rate measurement' _Sample_label $sample_4 save_ save_2D_1H-15N_HSQC_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_5 save_ save_2D_1H-15N_HSQC_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_6 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' 100 . mM pH 6.0 . pH pressure 1 . atm temperature 303 . K stop_ save_ save_sample_conditions_2 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 100 . mM pH 6.0 . pH pressure 1 . atm temperature 303 . K stop_ save_ save_sample_conditions_3 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 100 . mM pH 6.0 . pH pressure 1 . atm temperature 303 . K stop_ save_ save_sample_conditions_4 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 100 . mM pH 6.0 . pH pressure 1 . atm temperature 303 . K stop_ save_ save_sample_conditions_5 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 100 . mM pH 6.0 . pH pressure 1 . atm temperature 303 . K stop_ save_ save_sample_conditions_6 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 100 . mM pH 6.0 . pH pressure 1 . atm temperature 303 . 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 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_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' stop_ loop_ _Sample_label $sample_5 $sample_6 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_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 2 2 GLN H H 8.875 . . 2 2 2 GLN N N 123.090 . . 3 3 3 ILE H H 8.336 . . 4 3 3 ILE N N 115.317 . . 5 4 4 PHE H H 8.622 . . 6 4 4 PHE N N 118.705 . . 7 5 5 VAL H H 9.319 . . 8 5 5 VAL N N 121.503 . . 9 6 6 LYS H H 9.000 . . 10 6 6 LYS N N 128.142 . . 11 7 7 THR H H 8.744 . . 12 7 7 THR N N 115.457 . . 13 8 8 LEU H H 9.117 . . 14 8 8 LEU N N 121.449 . . 15 9 9 THR H H 7.656 . . 16 9 9 THR N N 126.497 . . 17 10 10 GLY H H 7.849 . . 18 10 10 GLY N N 109.346 . . 19 11 11 LYS H H 7.297 . . 20 11 11 LYS N N 122.051 . . 21 12 12 THR H H 8.629 . . 22 12 12 THR N N 120.723 . . 23 13 13 ILE H H 9.583 . . 24 13 13 ILE N N 127.909 . . 25 14 14 THR H H 8.728 . . 26 14 14 THR N N 121.861 . . 27 15 15 LEU H H 8.739 . . 28 15 15 LEU N N 125.293 . . 29 16 16 GLU H H 8.139 . . 30 16 16 GLU N N 122.763 . . 31 17 17 VAL H H 8.944 . . 32 17 17 VAL N N 117.729 . . 33 18 18 GLU H H 8.700 . . 34 18 18 GLU N N 119.594 . . 35 20 20 SER H H 7.050 . . 36 20 20 SER N N 124.154 . . 37 21 21 ASP H H 8.070 . . 38 21 21 ASP N N 124.036 . . 39 22 22 THR H H 7.886 . . 40 22 22 THR N N 109.090 . . 41 23 23 ILE H H 8.536 . . 42 23 23 ILE N N 121.455 . . 43 25 25 CYS H H 7.940 . . 44 25 25 CYS N N 121.510 . . 45 26 26 VAL H H 8.123 . . 46 26 26 VAL N N 122.322 . . 47 27 27 LYS H H 8.571 . . 48 27 27 LYS N N 119.098 . . 49 28 28 ALA H H 7.998 . . 50 28 28 ALA N N 123.566 . . 51 29 29 LYS H H 7.892 . . 52 29 29 LYS N N 120.388 . . 53 30 30 ILE H H 8.303 . . 54 30 30 ILE N N 121.472 . . 55 31 31 GLN H H 8.569 . . 56 31 31 GLN N N 123.713 . . 57 32 32 ASP H H 8.039 . . 58 32 32 ASP N N 119.932 . . 59 33 33 LYS H H 7.473 . . 60 33 33 LYS N N 115.669 . . 61 34 34 GLU H H 8.740 . . 62 34 34 GLU N N 114.495 . . 63 35 35 GLY H H 8.502 . . 64 35 35 GLY N N 108.947 . . 65 36 36 ILE H H 6.186 . . 66 36 36 ILE N N 120.438 . . 67 39 39 ASP H H 8.554 . . 68 39 39 ASP N N 113.748 . . 69 40 40 GLN H H 7.841 . . 70 40 40 GLN N N 117.015 . . 71 41 41 GLN H H 7.494 . . 72 41 41 GLN N N 118.149 . . 73 42 42 ARG H H 8.514 . . 74 42 42 ARG N N 123.178 . . 75 43 43 LEU H H 8.818 . . 76 43 43 LEU N N 124.593 . . 77 44 44 ILE H H 9.155 . . 78 44 44 ILE N N 122.637 . . 79 45 45 PHE H H 8.865 . . 80 45 45 PHE N N 125.152 . . 81 46 46 ALA H H 8.986 . . 82 46 46 ALA N N 112.473 . . 83 47 47 GLY H H 8.094 . . 84 47 47 GLY N N 123.105 . . 85 48 48 CYS H H 8.001 . . 86 48 48 CYS N N 122.066 . . 87 49 49 GLN H H 8.641 . . 88 49 49 GLN N N 123.249 . . 89 50 50 LEU H H 8.576 . . 90 50 50 LEU N N 125.854 . . 91 51 51 GLU H H 8.391 . . 92 51 51 GLU N N 123.307 . . 93 52 52 ASP H H 8.166 . . 94 52 52 ASP N N 120.548 . . 95 54 54 ARG H H 7.484 . . 96 54 54 ARG N N 119.451 . . 97 55 55 THR H H 8.854 . . 98 55 55 THR N N 109.015 . . 99 56 56 LEU H H 8.180 . . 100 56 56 LEU N N 118.234 . . 101 57 57 SER H H 8.485 . . 102 57 57 SER N N 113.618 . . 103 58 58 ASP H H 7.948 . . 104 58 58 ASP N N 124.626 . . 105 59 59 TYR H H 7.285 . . 106 59 59 TYR N N 115.893 . . 107 60 60 ASN H H 8.169 . . 108 60 60 ASN N N 116.048 . . 109 61 61 ILE H H 7.260 . . 110 61 61 ILE N N 119.076 . . 111 62 62 GLN H H 7.653 . . 112 62 62 GLN N N 125.061 . . 113 63 63 LYS H H 8.479 . . 114 63 63 LYS N N 120.622 . . 115 64 64 GLU H H 9.316 . . 116 64 64 GLU N N 115.279 . . 117 65 65 SER H H 7.742 . . 118 65 65 SER N N 115.102 . . 119 66 66 THR H H 8.699 . . 120 66 66 THR N N 117.565 . . 121 67 67 LEU H H 9.427 . . 122 67 67 LEU N N 127.940 . . 123 68 68 HIS H H 9.241 . . 124 68 68 HIS N N 119.784 . . 125 69 69 LEU H H 8.322 . . 126 69 69 LEU N N 124.014 . . 127 70 70 VAL H H 9.197 . . 128 70 70 VAL N N 127.016 . . 129 71 71 LEU H H 8.116 . . 130 71 71 LEU N N 123.344 . . 131 72 72 ARG H H 8.624 . . 132 72 72 ARG N N 123.792 . . 133 73 73 LEU H H 8.352 . . 134 73 73 LEU N N 124.467 . . 135 74 74 ARG H H 8.487 . . 136 74 74 ARG N N 122.301 . . 137 75 75 GLY H H 8.568 . . 138 75 75 GLY N N 111.035 . . 139 76 76 GLY H H 8.357 . . 140 76 76 GLY N N 109.384 . . stop_ save_ save_assigned_chem_shift_list_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' stop_ loop_ _Sample_label $sample_5 $sample_6 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name entity_2 _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 GLN H H 8.915 . . 2 2 2 GLN N N 123.219 . . 3 3 3 ILE H H 8.328 . . 4 3 3 ILE N N 115.369 . . 5 4 4 PHE H H 8.624 . . 6 4 4 PHE N N 118.697 . . 7 5 5 VAL H H 9.319 . . 8 5 5 VAL N N 121.481 . . 9 6 6 LYS H H 8.968 . . 10 6 6 LYS N N 128.092 . . 11 7 7 THR H H 8.751 . . 12 7 7 THR N N 115.578 . . 13 8 8 LEU H H 9.110 . . 14 8 8 LEU N N 121.483 . . 15 9 9 THR H H 7.658 . . 16 9 9 THR N N 126.534 . . 17 10 10 GLY H H 7.846 . . 18 10 10 GLY N N 109.339 . . 19 11 11 LYS H H 7.294 . . 20 11 11 LYS N N 122.047 . . 21 12 12 THR H H 8.634 . . 22 12 12 THR N N 120.746 . . 23 13 13 ILE H H 9.563 . . 24 13 13 ILE N N 127.784 . . 25 14 14 THR H H 8.729 . . 26 14 14 THR N N 121.832 . . 27 15 15 LEU H H 8.744 . . 28 15 15 LEU N N 125.275 . . 29 16 16 GLU H H 8.144 . . 30 16 16 GLU N N 122.731 . . 31 17 17 VAL H H 8.936 . . 32 17 17 VAL N N 117.712 . . 33 18 18 GLU H H 8.700 . . 34 18 18 GLU N N 119.592 . . 35 20 20 SER H H 7.048 . . 36 20 20 SER N N 124.154 . . 37 21 21 ASP H H 8.063 . . 38 21 21 ASP N N 124.011 . . 39 22 22 THR H H 7.886 . . 40 22 22 THR N N 109.100 . . 41 23 23 ILE H H 8.541 . . 42 23 23 ILE N N 121.495 . . 43 25 25 ASN H H 7.941 . . 44 25 25 ASN N N 121.457 . . 45 26 26 VAL H H 8.122 . . 46 26 26 VAL N N 122.314 . . 47 27 27 LYS H H 8.573 . . 48 27 27 LYS N N 119.112 . . 49 28 28 ALA H H 8.004 . . 50 28 28 ALA N N 123.579 . . 51 29 29 LYS H H 7.887 . . 52 29 29 LYS N N 120.374 . . 53 30 30 ILE H H 8.299 . . 54 30 30 ILE N N 121.472 . . 55 31 31 GLN H H 8.572 . . 56 31 31 GLN N N 123.726 . . 57 32 32 ASP H H 8.038 . . 58 32 32 ASP N N 119.925 . . 59 33 33 LYS H H 7.472 . . 60 33 33 LYS N N 115.659 . . 61 34 34 GLU H H 8.743 . . 62 34 34 GLU N N 114.499 . . 63 35 35 GLY H H 8.511 . . 64 35 35 GLY N N 109.001 . . 65 36 36 ILE H H 6.182 . . 66 36 36 ILE N N 120.450 . . 67 39 39 ASP H H 8.545 . . 68 39 39 ASP N N 113.721 . . 69 40 40 GLN H H 7.828 . . 70 40 40 GLN N N 116.994 . . 71 41 41 GLN H H 7.487 . . 72 41 41 GLN N N 118.118 . . 73 42 42 ARG H H 8.531 . . 74 42 42 ARG N N 123.193 . . 75 43 43 LEU H H 8.821 . . 76 43 43 LEU N N 124.581 . . 77 44 44 ILE H H 9.136 . . 78 44 44 ILE N N 122.572 . . 79 45 45 PHE H H 8.858 . . 80 45 45 PHE N N 125.248 . . 81 46 46 ALA H H 8.947 . . 82 46 46 ALA N N 112.377 . . 83 47 47 GLY H H 8.105 . . 84 47 47 GLY N N 123.094 . . 85 48 48 LYS H H 7.995 . . 86 48 48 LYS N N 122.056 . . 87 49 49 GLN H H 8.637 . . 88 49 49 GLN N N 123.168 . . 89 50 50 LEU H H 8.580 . . 90 50 50 LEU N N 125.834 . . 91 51 51 GLU H H 8.399 . . 92 51 51 GLU N N 123.329 . . 93 52 52 ASP H H 8.170 . . 94 52 52 ASP N N 120.565 . . 95 54 54 ARG H H 7.489 . . 96 54 54 ARG N N 119.478 . . 97 55 55 THR H H 8.849 . . 98 55 55 THR N N 109.001 . . 99 56 56 LEU H H 8.172 . . 100 56 56 LEU N N 118.246 . . 101 57 57 SER H H 8.472 . . 102 57 57 SER N N 113.579 . . 103 58 58 ASP H H 7.952 . . 104 58 58 ASP N N 124.650 . . 105 59 59 TYR H H 7.281 . . 106 59 59 TYR N N 115.888 . . 107 60 60 ASN H H 8.171 . . 108 60 60 ASN N N 116.035 . . 109 61 61 ILE H H 7.254 . . 110 61 61 ILE N N 119.008 . . 111 62 62 GLN H H 7.632 . . 112 62 62 GLN N N 125.173 . . 113 63 63 LYS H H 8.415 . . 114 63 63 LYS N N 121.083 . . 115 64 64 GLU H H 9.257 . . 116 64 64 GLU N N 114.474 . . 117 65 65 SER H H 7.705 . . 118 65 65 SER N N 115.014 . . 119 66 66 THR H H 8.709 . . 120 66 66 THR N N 117.578 . . 121 67 67 LEU H H 9.428 . . 122 67 67 LEU N N 127.831 . . 123 68 68 HIS H H 9.244 . . 124 68 68 HIS N N 119.560 . . 125 69 69 LEU H H 8.325 . . 126 69 69 LEU N N 124.170 . . 127 70 70 VAL H H 9.198 . . 128 70 70 VAL N N 127.020 . . 129 71 71 LEU H H 8.105 . . 130 71 71 LEU N N 123.391 . . stop_ save_