data_15708 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Structure of the N-terminal domain of the Y4 receptor in SDS and DPC micelles ; _BMRB_accession_number 15708 _BMRB_flat_file_name bmr15708.str _Entry_type original _Submission_date 2008-04-02 _Accession_date 2008-04-02 _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 Zou Chao . . 2 Kumaran Sowmini . . 3 Reto Walser . . 4 Markovic Stefan . . 5 Zerbe Oliver . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 heteronucl_NOE 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 457 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2010-06-02 update BMRB 'edit assembly name' 2008-12-15 update BMRB 'complete entry citation' 2008-09-11 original author 'original release' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Studies of the Structure of the N-Terminal Domain from the Y4 Receptor-a G Protein-Coupled Receptor-and its Interaction with Hormones from the NPY Family' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 18767100 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Zou Chao . . 2 Kumaran Sowmini . . 3 Markovic Stefan . . 4 Walser Reto . . 5 Zerbe Oliver . . stop_ _Journal_abbreviation ChemBioChem _Journal_volume 9 _Journal_issue 14 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 2276 _Page_last 2284 _Year 2008 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name N-terminal_domain_of_Y4_receptor _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label entity $N-terminal_domain_of_Y4_receptor 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_N-terminal_domain_of_Y4_receptor _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common N-terminal_domain_of_Y4_receptor _Molecular_mass 4561.191 _Mol_thiol_state 'not present' loop_ _Biological_function 'GPCR fragment' stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 41 _Mol_residue_sequence ; MNTSHLLALLLPKSPQGENR SKPLGTPYNFSEHCQDSVDV M ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 MET 2 2 ASN 3 3 THR 4 4 SER 5 5 HIS 6 6 LEU 7 7 LEU 8 8 ALA 9 9 LEU 10 10 LEU 11 11 LEU 12 12 PRO 13 13 LYS 14 14 SER 15 15 PRO 16 16 GLN 17 17 GLY 18 18 GLU 19 19 ASN 20 20 ARG 21 21 SER 22 22 LYS 23 23 PRO 24 24 LEU 25 25 GLY 26 26 THR 27 27 PRO 28 28 TYR 29 29 ASN 30 30 PHE 31 31 SER 32 32 GLU 33 33 HIS 34 34 CYS 35 35 GLN 36 36 ASP 37 37 SER 38 38 VAL 39 39 ASP 40 40 VAL 41 41 MET stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2015-07-08 loop_ _Database_name _Database_accession_code _Database_entry_mol_name _Sequence_query_to_submitted_percentage _Sequence_subject_length _Sequence_identity _Sequence_positive _Sequence_homology_expectation_value BMRB 15921 N-TM1-TM2 100.00 121 100.00 100.00 8.20e-21 BMRB 18319 Y4_TM1-TM2 100.00 121 100.00 100.00 8.20e-21 DBJ BAG74162 "pancreatic polypeptide receptor 1 [synthetic construct]" 100.00 375 100.00 100.00 5.79e-20 EMBL CAA91433 "pancreatic polypeptide receptor PP1 [Homo sapiens]" 100.00 375 100.00 100.00 5.79e-20 EMBL CAG46748 "PPYR1 [Homo sapiens]" 100.00 375 100.00 100.00 5.91e-20 EMBL CAI13318 "pancreatic polypeptide receptor 1 [Homo sapiens]" 100.00 375 100.00 100.00 5.79e-20 GB AAB07759 "pancreatic polypeptide receptor [Homo sapiens]" 100.00 375 100.00 100.00 6.03e-20 GB AAC50280 "neuropeptide Y4 receptor protein [Homo sapiens]" 100.00 375 100.00 100.00 5.79e-20 GB AAH96238 "Pancreatic polypeptide receptor 1 [Homo sapiens]" 100.00 375 100.00 100.00 6.03e-20 GB AAH99637 "Pancreatic polypeptide receptor 1 [Homo sapiens]" 100.00 375 100.00 100.00 5.97e-20 GB AAP23199 "pancreatic polypeptide receptor 1 [Homo sapiens]" 100.00 375 100.00 100.00 5.79e-20 REF NP_001265723 "neuropeptide Y receptor type 4 [Homo sapiens]" 100.00 375 100.00 100.00 5.91e-20 REF NP_001265724 "neuropeptide Y receptor type 4-like [Homo sapiens]" 100.00 375 100.00 100.00 5.79e-20 REF NP_005963 "neuropeptide Y receptor type 4 [Homo sapiens]" 100.00 375 100.00 100.00 5.91e-20 REF XP_003804406 "PREDICTED: neuropeptide Y receptor type 4 [Pan paniscus]" 100.00 375 97.56 100.00 2.19e-19 REF XP_003804407 "PREDICTED: neuropeptide Y receptor type 4 [Pan paniscus]" 100.00 375 97.56 100.00 2.19e-19 SP P50391 "RecName: Full=Neuropeptide Y receptor type 4; Short=NPY4-R; AltName: Full=Pancreatic polypeptide receptor 1; Short=PP1" 100.00 375 100.00 100.00 5.79e-20 stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $N-terminal_domain_of_Y4_receptor 'E. coli' 562 Eubacteria . Escherichia coli 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 _Details $N-terminal_domain_of_Y4_receptor 'recombinant technology' . Escherichia coli BL21 C43 pET 'KSI fusion vector' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details 'in the presence of SDS micelles' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $N-terminal_domain_of_Y4_receptor 1 mM 'natural abundance' MES 40 mM 'natural abundance' SDS 300 mM 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details 'in the presence of DPC micelles' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $N-terminal_domain_of_Y4_receptor 1 mM 'natural abundance' MES 40 mM 'natural abundance' DPC 300 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_XEASY_CARA _Saveframe_category software _Name XEASY/CARA _Version 1.5 loop_ _Vendor _Address _Electronic_address 'Bartels et al.' . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 700 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_TOCSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_3D_1H-15N_NOESY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N NOESY' _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_2 save_ save_2D_1H-15N_HSQC_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_2 save_ save_2D_1H-1H_NOESY_7 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_2 save_ save_3D_1H-15N_NOESY_8 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N NOESY' _Sample_label $sample_2 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details 'measurement in micelles' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0 . M pH 5.6 0.2 pH pressure 1 . atm temperature 310 1 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 _Indirect_shift_ratio_citation_label _Correction_value_citation_label water H 1 protons ppm 4.63 internal direct . . . 1.0 $entry_citation $entry_citation 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 'chemical shifts are referenced to the water position at 4.63 ppm at 310K' loop_ _Software_label $XEASY_CARA stop_ loop_ _Experiment_label '2D 1H-1H NOESY' 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 entity _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 MET HA H 4.191 0.002 1 2 1 1 MET HB2 H 2.187 0.006 1 3 1 1 MET HB3 H 2.187 0.006 1 4 1 1 MET HG2 H 2.547 0.002 1 5 1 1 MET HG3 H 2.547 0.002 1 6 2 2 ASN H H 8.659 0.002 1 7 2 2 ASN HA H 4.976 0.001 1 8 2 2 ASN HB2 H 2.979 0.004 2 9 2 2 ASN HB3 H 2.790 0.007 2 10 2 2 ASN HD21 H 7.571 0.003 2 11 2 2 ASN HD22 H 6.860 0.002 2 12 3 3 THR H H 8.289 0.006 1 13 3 3 THR HA H 4.263 0.005 1 14 3 3 THR HB H 4.039 0.005 1 15 3 3 THR HG2 H 1.218 0.004 1 16 4 4 SER H H 8.287 0.003 1 17 4 4 SER HA H 4.226 0.005 1 18 4 4 SER HB2 H 3.924 0.003 1 19 4 4 SER HB3 H 3.924 0.003 1 20 5 5 HIS H H 8.065 0.005 1 21 5 5 HIS HA H 4.565 0.003 1 22 5 5 HIS HB2 H 3.302 0.005 1 23 5 5 HIS HB3 H 3.302 0.005 1 24 5 5 HIS HD2 H 7.341 0.001 1 25 5 5 HIS HE1 H 8.646 0.003 1 26 6 6 LEU H H 7.843 0.003 1 27 6 6 LEU HA H 4.001 0.004 1 28 6 6 LEU HB2 H 1.695 0.008 2 29 6 6 LEU HB3 H 1.786 0.008 2 30 6 6 LEU HD1 H 0.869 0.005 2 31 6 6 LEU HD2 H 0.937 0.003 2 32 6 6 LEU HG H 1.574 0.010 1 33 7 7 LEU H H 8.029 0.004 1 34 7 7 LEU HA H 3.956 0.004 1 35 7 7 LEU HB2 H 1.572 0.008 2 36 7 7 LEU HB3 H 1.779 0.006 2 37 7 7 LEU HD1 H 0.867 0.003 2 38 7 7 LEU HD2 H 0.933 0.006 2 39 7 7 LEU HG H 1.579 0.009 1 40 8 8 ALA H H 7.523 0.004 1 41 8 8 ALA HA H 4.047 0.006 1 42 8 8 ALA HB H 1.467 0.005 1 43 9 9 LEU H H 7.473 0.003 1 44 9 9 LEU HA H 4.142 0.005 1 45 9 9 LEU HB2 H 1.705 0.003 2 46 9 9 LEU HB3 H 1.872 0.003 2 47 9 9 LEU HD1 H 0.861 0.005 2 48 9 9 LEU HD2 H 0.937 0.006 2 49 9 9 LEU HG H 1.540 0.009 1 50 10 10 LEU H H 7.597 0.004 1 51 10 10 LEU HA H 4.218 0.003 1 52 10 10 LEU HB2 H 1.753 0.008 2 53 10 10 LEU HB3 H 1.803 0.008 2 54 10 10 LEU HD1 H 0.819 0.001 2 55 10 10 LEU HD2 H 0.863 0.002 2 56 10 10 LEU HG H 1.553 0.006 1 57 11 11 LEU H H 7.655 0.003 1 58 11 11 LEU HA H 4.366 0.002 1 59 11 11 LEU HB2 H 1.774 0.009 1 60 11 11 LEU HB3 H 1.774 0.009 1 61 11 11 LEU HD1 H 0.901 0.004 2 62 11 11 LEU HD2 H 0.937 0.005 2 63 11 11 LEU HG H 1.560 0.007 1 64 12 12 PRO HB2 H 1.705 0.003 1 65 12 12 PRO HB3 H 1.705 0.003 1 66 12 12 PRO HD2 H 3.546 0.004 2 67 12 12 PRO HD3 H 3.768 0.006 2 68 13 13 LYS H H 7.902 0.003 1 69 13 13 LYS HA H 4.444 0.001 1 70 13 13 LYS HB2 H 1.806 0.004 1 71 13 13 LYS HB3 H 1.806 0.004 1 72 13 13 LYS HG2 H 1.462 0.005 1 73 13 13 LYS HG3 H 1.462 0.005 1 74 13 13 LYS HZ H 6.960 0.003 1 75 14 14 SER H H 7.950 0.001 1 76 14 14 SER HA H 3.877 0.003 1 77 14 14 SER HB2 H 3.800 0.003 1 78 14 14 SER HB3 H 3.800 0.003 1 79 15 15 PRO HA H 4.455 0.001 1 80 15 15 PRO HD2 H 3.746 0.005 2 81 15 15 PRO HD3 H 3.798 0.004 2 82 16 16 GLN H H 8.284 0.002 1 83 16 16 GLN HA H 4.308 0.002 1 84 16 16 GLN HB2 H 1.972 0.002 2 85 16 16 GLN HB3 H 2.150 0.002 2 86 16 16 GLN HE21 H 7.426 0.003 2 87 16 16 GLN HE22 H 6.727 0.003 2 88 16 16 GLN HG2 H 2.305 0.001 2 89 16 16 GLN HG3 H 2.371 0.001 2 90 17 17 GLY H H 8.182 0.002 1 91 17 17 GLY HA2 H 3.931 0.001 1 92 17 17 GLY HA3 H 3.931 0.001 1 93 18 18 GLU H H 8.141 0.004 1 94 18 18 GLU HA H 4.302 0.006 1 95 18 18 GLU HB2 H 1.943 0.009 2 96 18 18 GLU HB3 H 2.077 0.001 2 97 18 18 GLU HG2 H 2.329 0.007 1 98 18 18 GLU HG3 H 2.329 0.007 1 99 19 19 ASN H H 8.302 0.006 1 100 19 19 ASN HA H 4.706 0.003 1 101 19 19 ASN HB2 H 2.711 0.004 2 102 19 19 ASN HB3 H 2.836 0.001 2 103 19 19 ASN HD21 H 7.495 0.003 2 104 19 19 ASN HD22 H 6.838 0.002 2 105 20 20 ARG H H 7.989 0.003 1 106 20 20 ARG HA H 4.353 0.001 1 107 20 20 ARG HB2 H 1.778 0.007 2 108 20 20 ARG HB3 H 1.862 0.007 2 109 20 20 ARG HD2 H 3.193 0.004 1 110 20 20 ARG HD3 H 3.193 0.004 1 111 20 20 ARG HE H 7.186 0.003 1 112 20 20 ARG HG2 H 1.646 0.008 1 113 20 20 ARG HG3 H 1.646 0.008 1 114 21 21 SER H H 8.220 0.003 1 115 21 21 SER HA H 4.434 0.001 1 116 21 21 SER HB2 H 3.828 0.005 1 117 21 21 SER HB3 H 3.828 0.005 1 118 22 22 LYS H H 7.998 0.004 1 119 22 22 LYS HA H 4.348 0.002 1 120 22 22 LYS HB2 H 1.747 0.004 1 121 22 22 LYS HB3 H 1.747 0.004 1 122 22 22 LYS HG2 H 1.456 0.012 1 123 22 22 LYS HG3 H 1.456 0.012 1 124 23 23 PRO HA H 4.441 0.008 1 125 23 23 PRO HB2 H 1.984 0.006 2 126 23 23 PRO HB3 H 2.306 0.005 2 127 23 23 PRO HD2 H 3.677 0.004 2 128 23 23 PRO HD3 H 3.772 0.002 2 129 23 23 PRO HG2 H 1.910 0.003 1 130 23 23 PRO HG3 H 1.910 0.003 1 131 24 24 LEU H H 8.034 0.003 1 132 24 24 LEU HA H 4.337 0.001 1 133 24 24 LEU HB2 H 1.676 0.002 2 134 24 24 LEU HB3 H 1.719 0.001 2 135 24 24 LEU HD1 H 0.884 0.003 1 136 24 24 LEU HD2 H 0.884 0.003 1 137 25 25 GLY H H 7.974 0.009 1 138 25 25 GLY HA2 H 3.915 0.001 2 139 25 25 GLY HA3 H 4.003 0.003 2 140 26 26 THR H H 7.820 0.002 1 141 26 26 THR HA H 4.611 0.003 1 142 26 26 THR HB H 4.170 0.010 1 143 26 26 THR HG2 H 1.211 0.004 1 144 27 27 PRO HA H 4.390 0.002 1 145 27 27 PRO HB2 H 2.174 0.007 1 146 27 27 PRO HB3 H 2.174 0.007 1 147 27 27 PRO HG2 H 2.167 0.003 1 148 27 27 PRO HG3 H 2.167 0.003 1 149 28 28 TYR H H 7.614 0.005 1 150 28 28 TYR HA H 4.338 0.002 1 151 28 28 TYR HB2 H 2.642 0.007 2 152 28 28 TYR HB3 H 2.715 0.005 2 153 28 28 TYR HD1 H 6.881 0.003 1 154 28 28 TYR HD2 H 6.881 0.003 1 155 28 28 TYR HE1 H 6.709 0.004 1 156 28 28 TYR HE2 H 6.709 0.004 1 157 29 29 ASN H H 7.930 0.006 1 158 29 29 ASN HA H 4.678 0.001 1 159 29 29 ASN HB2 H 2.630 0.008 2 160 29 29 ASN HB3 H 2.800 0.004 2 161 29 29 ASN HD21 H 7.429 0.003 2 162 29 29 ASN HD22 H 6.760 0.002 2 163 30 30 PHE H H 8.079 0.005 1 164 30 30 PHE HA H 4.426 0.001 1 165 30 30 PHE HB2 H 3.067 0.006 2 166 30 30 PHE HB3 H 3.187 0.004 2 167 30 30 PHE HD1 H 7.281 0.003 1 168 30 30 PHE HD2 H 7.281 0.003 1 169 30 30 PHE HE1 H 7.217 0.004 1 170 30 30 PHE HE2 H 7.217 0.004 1 171 30 30 PHE HZ H 7.071 0.006 1 172 31 31 SER H H 8.186 0.006 1 173 31 31 SER HA H 4.309 0.003 1 174 31 31 SER HB2 H 3.878 0.008 1 175 31 31 SER HB3 H 3.878 0.008 1 176 32 32 GLU H H 7.848 0.007 1 177 32 32 GLU HA H 4.232 0.001 1 178 32 32 GLU HB2 H 1.913 0.009 2 179 32 32 GLU HB3 H 2.028 0.003 2 180 32 32 GLU HG2 H 2.295 0.006 1 181 32 32 GLU HG3 H 2.295 0.006 1 182 33 33 HIS H H 8.124 0.004 1 183 33 33 HIS HA H 4.626 0.007 1 184 33 33 HIS HB2 H 3.197 0.006 2 185 33 33 HIS HB3 H 3.341 0.003 2 186 33 33 HIS HD2 H 7.316 0.003 1 187 34 34 CYS H H 8.158 0.002 1 188 34 34 CYS HA H 4.660 0.001 1 189 34 34 CYS HB2 H 3.218 0.004 2 190 34 34 CYS HB3 H 2.981 0.006 2 191 35 35 GLN H H 8.245 0.007 1 192 35 35 GLN HA H 4.334 0.001 1 193 35 35 GLN HB2 H 1.984 0.007 2 194 35 35 GLN HB3 H 2.110 0.005 2 195 35 35 GLN HE21 H 7.417 0.003 2 196 35 35 GLN HE22 H 6.755 0.003 2 197 35 35 GLN HG2 H 2.345 0.003 1 198 35 35 GLN HG3 H 2.345 0.003 1 199 36 36 ASP H H 8.314 0.002 1 200 36 36 ASP HA H 4.650 0.003 1 201 36 36 ASP HB2 H 2.696 0.003 2 202 36 36 ASP HB3 H 2.756 0.004 2 203 37 37 SER H H 8.182 0.006 1 204 37 37 SER HA H 4.454 0.002 1 205 37 37 SER HB2 H 3.848 0.004 1 206 37 37 SER HB3 H 3.848 0.004 1 207 38 38 VAL H H 7.990 0.007 1 208 38 38 VAL HA H 4.143 0.003 1 209 38 38 VAL HB H 2.086 0.004 1 210 38 38 VAL HG1 H 0.847 0.003 2 211 38 38 VAL HG2 H 0.889 0.003 2 212 39 39 ASP H H 8.295 0.004 1 213 39 39 ASP HA H 4.620 0.003 1 214 39 39 ASP HB2 H 2.595 0.007 1 215 39 39 ASP HB3 H 2.595 0.007 1 216 40 40 VAL H H 7.947 0.006 1 217 40 40 VAL HA H 4.116 0.005 1 218 40 40 VAL HB H 2.092 0.003 1 219 40 40 VAL HG1 H 0.898 0.002 1 220 40 40 VAL HG2 H 0.898 0.002 1 221 41 41 MET H H 7.898 0.003 1 222 41 41 MET HA H 4.344 0.003 1 223 41 41 MET HB2 H 1.921 0.003 2 224 41 41 MET HB3 H 1.912 0.003 2 225 41 41 MET HG2 H 2.341 0.003 1 226 41 41 MET HG3 H 2.341 0.003 1 stop_ save_ save_assigned_chem_shift_list_2 _Saveframe_category assigned_chemical_shifts _Details 'chemical shifts are referenced to the water position at 4.63 ppm at 310K' loop_ _Software_label $XEASY_CARA stop_ loop_ _Experiment_label '2D 1H-1H NOESY' stop_ loop_ _Sample_label $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name entity _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 MET HA H 4.071 0.003 1 2 2 2 ASN H H 8.990 0.005 1 3 2 2 ASN HA H 4.920 0.004 1 4 2 2 ASN HB2 H 2.920 0.003 2 5 2 2 ASN HB3 H 2.800 0.003 2 6 2 2 ASN HD21 H 7.660 0.003 2 7 2 2 ASN HD22 H 6.900 0.003 2 8 3 3 THR H H 8.630 0.002 1 9 3 3 THR HA H 3.890 0.001 1 10 3 3 THR HB H 4.200 0.003 1 11 3 3 THR HG2 H 1.198 0.003 1 12 4 4 SER H H 8.430 0.002 1 13 4 4 SER HA H 4.137 0.003 1 14 4 4 SER HB2 H 3.905 0.001 1 15 4 4 SER HB3 H 3.905 0.001 1 16 5 5 HIS H H 8.108 0.004 1 17 5 5 HIS HA H 4.502 0.003 1 18 5 5 HIS HB2 H 3.250 0.001 1 19 5 5 HIS HB3 H 3.250 0.001 1 20 5 5 HIS HD2 H 6.890 0.003 1 21 5 5 HIS HE1 H 7.660 0.003 1 22 6 6 LEU H H 7.688 0.002 1 23 6 6 LEU HA H 3.984 0.002 1 24 6 6 LEU HB2 H 1.743 0.003 1 25 6 6 LEU HB3 H 1.743 0.003 1 26 6 6 LEU HD1 H 0.896 0.003 2 27 6 6 LEU HD2 H 0.839 0.003 2 28 6 6 LEU HG H 1.670 0.009 1 29 7 7 LEU H H 8.011 0.003 1 30 7 7 LEU HA H 3.913 0.003 1 31 7 7 LEU HB2 H 1.755 0.003 1 32 7 7 LEU HB3 H 1.755 0.003 1 33 7 7 LEU HD1 H 0.850 0.003 1 34 7 7 LEU HD2 H 0.850 0.003 1 35 7 7 LEU HG H 1.580 0.007 1 36 8 8 ALA H H 7.522 0.003 1 37 8 8 ALA HA H 4.031 0.003 1 38 8 8 ALA HB H 1.440 0.003 1 39 9 9 LEU H H 7.398 0.002 1 40 9 9 LEU HA H 4.092 0.003 1 41 9 9 LEU HB2 H 1.889 0.003 1 42 9 9 LEU HB3 H 1.889 0.003 1 43 9 9 LEU HD1 H 0.829 0.003 1 44 9 9 LEU HD2 H 0.829 0.003 1 45 9 9 LEU HG H 1.470 0.014 1 46 10 10 LEU H H 7.428 0.005 1 47 10 10 LEU HA H 4.192 0.003 1 48 10 10 LEU HB2 H 1.720 0.003 1 49 10 10 LEU HB3 H 1.720 0.003 1 50 10 10 LEU HD1 H 0.830 0.035 2 51 10 10 LEU HD2 H 0.790 0.029 2 52 10 10 LEU HG H 1.558 0.010 1 53 11 11 LEU H H 7.496 0.001 1 54 11 11 LEU HA H 4.513 0.003 1 55 11 11 LEU HB2 H 1.654 0.002 1 56 11 11 LEU HB3 H 1.654 0.002 1 57 11 11 LEU HD1 H 0.870 0.003 1 58 11 11 LEU HD2 H 0.870 0.003 1 59 11 11 LEU HG H 1.505 0.003 1 60 12 12 PRO HB2 H 2.290 0.003 2 61 12 12 PRO HB3 H 1.860 0.003 2 62 12 12 PRO HD2 H 3.540 0.003 2 63 12 12 PRO HD3 H 3.690 0.003 2 64 13 13 LYS H H 8.350 0.002 1 65 13 13 LYS HA H 4.300 0.003 1 66 13 13 LYS HB2 H 1.700 0.001 1 67 13 13 LYS HB3 H 1.700 0.001 1 68 13 13 LYS HD2 H 1.780 0.003 1 69 13 13 LYS HD3 H 1.780 0.003 1 70 13 13 LYS HE2 H 2.960 0.003 1 71 13 13 LYS HE3 H 2.960 0.003 1 72 13 13 LYS HG2 H 1.420 0.003 1 73 13 13 LYS HG3 H 1.420 0.003 1 74 14 14 SER H H 8.300 0.003 1 75 14 14 SER HA H 4.680 0.003 1 76 14 14 SER HB2 H 3.808 0.003 1 77 14 14 SER HB3 H 3.808 0.003 1 78 15 15 PRO HA H 4.402 0.003 1 79 15 15 PRO HB2 H 2.240 0.003 2 80 15 15 PRO HB3 H 1.880 0.003 2 81 15 15 PRO HD2 H 3.690 0.003 2 82 15 15 PRO HD3 H 3.790 0.003 2 83 15 15 PRO HG2 H 1.970 0.003 1 84 15 15 PRO HG3 H 1.970 0.003 1 85 16 16 GLN H H 8.364 0.005 1 86 16 16 GLN HA H 4.269 0.003 1 87 16 16 GLN HB2 H 2.080 0.009 2 88 16 16 GLN HB3 H 1.941 0.013 2 89 16 16 GLN HE21 H 7.450 0.003 2 90 16 16 GLN HE22 H 6.780 0.003 2 91 16 16 GLN HG2 H 2.330 0.003 1 92 16 16 GLN HG3 H 2.330 0.003 1 93 17 17 GLY H H 8.272 0.004 1 94 17 17 GLY HA2 H 3.905 0.001 1 95 17 17 GLY HA3 H 3.905 0.001 1 96 18 18 GLU H H 8.220 0.002 1 97 18 18 GLU HA H 4.255 0.001 1 98 18 18 GLU HB2 H 2.006 0.003 2 99 18 18 GLU HB3 H 1.880 0.003 2 100 18 18 GLU HG2 H 2.240 0.002 1 101 18 18 GLU HG3 H 2.240 0.002 1 102 19 19 ASN H H 8.450 0.008 1 103 19 19 ASN HA H 4.640 0.002 1 104 19 19 ASN HB2 H 2.791 0.003 2 105 19 19 ASN HB3 H 2.710 0.003 2 106 19 19 ASN HD21 H 7.530 0.003 2 107 19 19 ASN HD22 H 6.860 0.003 2 108 20 20 ARG H H 8.260 0.001 1 109 20 20 ARG HA H 4.310 0.001 1 110 20 20 ARG HB2 H 1.848 0.003 2 111 20 20 ARG HB3 H 1.710 0.003 2 112 20 20 ARG HD2 H 3.137 0.009 1 113 20 20 ARG HD3 H 3.137 0.009 1 114 20 20 ARG HG2 H 1.580 0.004 1 115 20 20 ARG HG3 H 1.580 0.004 1 116 21 21 SER H H 8.216 0.002 1 117 21 21 SER HA H 4.369 0.003 1 118 21 21 SER HB2 H 3.800 0.003 1 119 21 21 SER HB3 H 3.800 0.003 1 120 22 22 LYS H H 8.101 0.002 1 121 22 22 LYS HA H 4.570 0.003 1 122 22 22 LYS HB2 H 1.650 0.003 1 123 22 22 LYS HB3 H 1.650 0.003 1 124 22 22 LYS HD2 H 1.410 0.003 1 125 22 22 LYS HD3 H 1.410 0.003 1 126 22 22 LYS HE2 H 2.950 0.003 1 127 22 22 LYS HE3 H 2.950 0.003 1 128 22 22 LYS HG2 H 1.760 0.003 1 129 22 22 LYS HG3 H 1.760 0.003 1 130 23 23 PRO HA H 4.400 0.003 1 131 23 23 PRO HB2 H 2.270 0.003 1 132 23 23 PRO HB3 H 2.270 0.003 1 133 23 23 PRO HD2 H 3.550 0.003 1 134 23 23 PRO HD3 H 3.550 0.003 1 135 23 23 PRO HG2 H 1.980 0.003 1 136 23 23 PRO HG3 H 1.980 0.003 1 137 24 24 LEU H H 8.340 0.003 1 138 24 24 LEU HA H 4.264 0.003 1 139 24 24 LEU HB2 H 1.629 0.003 1 140 24 24 LEU HB3 H 1.629 0.003 1 141 24 24 LEU HD1 H 0.860 0.003 1 142 24 24 LEU HD2 H 0.860 0.003 1 143 24 24 LEU HG H 1.546 0.003 1 144 25 25 GLY H H 8.271 0.002 1 145 25 25 GLY HA2 H 3.918 0.003 1 146 25 25 GLY HA3 H 3.918 0.003 1 147 26 26 THR H H 7.941 0.002 1 148 26 26 THR HA H 4.533 0.003 1 149 26 26 THR HB H 4.080 0.003 1 150 26 26 THR HG2 H 1.144 0.003 1 151 27 27 PRO HB2 H 2.470 0.003 2 152 27 27 PRO HB3 H 2.140 0.003 2 153 27 27 PRO HD2 H 3.750 0.003 2 154 27 27 PRO HD3 H 3.570 0.003 2 155 27 27 PRO HG2 H 1.960 0.003 2 156 27 27 PRO HG3 H 1.820 0.003 2 157 28 28 TYR H H 7.910 0.012 1 158 28 28 TYR HA H 4.342 0.003 1 159 28 28 TYR HB2 H 2.788 0.004 1 160 28 28 TYR HB3 H 2.788 0.004 1 161 28 28 TYR HD1 H 6.918 0.004 1 162 28 28 TYR HD2 H 6.918 0.004 1 163 28 28 TYR HE1 H 6.714 0.003 1 164 28 28 TYR HE2 H 6.714 0.003 1 165 29 29 ASN H H 8.080 0.010 1 166 29 29 ASN HA H 4.610 0.004 1 167 29 29 ASN HB2 H 2.708 0.008 2 168 29 29 ASN HB3 H 2.589 0.004 2 169 29 29 ASN HD21 H 7.480 0.003 2 170 29 29 ASN HD22 H 6.790 0.003 2 171 30 30 PHE H H 8.210 0.044 1 172 30 30 PHE HA H 4.440 0.003 1 173 30 30 PHE HB2 H 3.130 0.003 2 174 30 30 PHE HB3 H 3.050 0.003 2 175 30 30 PHE HD1 H 7.240 0.003 1 176 30 30 PHE HD2 H 7.240 0.003 1 177 30 30 PHE HE1 H 7.140 0.003 1 178 30 30 PHE HE2 H 7.140 0.003 1 179 31 31 SER H H 8.071 0.007 1 180 31 31 SER HA H 4.391 0.001 1 181 31 31 SER HB2 H 3.813 0.003 1 182 31 31 SER HB3 H 3.813 0.003 1 183 32 32 GLU H H 8.080 0.025 1 184 32 32 GLU HA H 4.160 0.131 1 185 32 32 GLU HB2 H 1.940 0.019 2 186 32 32 GLU HB3 H 1.850 0.001 2 187 32 32 GLU HG2 H 2.210 0.012 1 188 32 32 GLU HG3 H 2.210 0.012 1 189 33 33 HIS H H 8.240 0.050 1 190 33 33 HIS HA H 4.590 0.168 1 191 33 33 HIS HB2 H 3.280 0.020 2 192 33 33 HIS HB3 H 3.090 0.008 2 193 34 34 CYS H H 8.200 0.106 1 194 34 34 CYS HA H 4.390 0.137 1 195 34 34 CYS HB2 H 2.855 0.003 1 196 34 34 CYS HB3 H 2.855 0.003 1 197 35 35 GLN H H 8.430 0.031 1 198 35 35 GLN HA H 4.250 0.031 1 199 35 35 GLN HB2 H 2.080 0.013 2 200 35 35 GLN HB3 H 1.960 0.009 2 201 35 35 GLN HE21 H 7.430 0.003 2 202 35 35 GLN HE22 H 6.760 0.003 2 203 35 35 GLN HG2 H 2.310 0.008 1 204 35 35 GLN HG3 H 2.310 0.008 1 205 36 36 ASP H H 8.250 0.037 1 206 36 36 ASP HA H 4.640 0.165 1 207 36 36 ASP HB2 H 2.760 0.022 2 208 36 36 ASP HB3 H 2.640 0.007 2 209 37 37 SER H H 8.130 0.010 1 210 37 37 SER HA H 4.420 0.092 1 211 37 37 SER HB2 H 3.795 0.005 1 212 37 37 SER HB3 H 3.795 0.005 1 213 38 38 VAL H H 8.005 0.002 1 214 38 38 VAL HA H 4.109 0.002 1 215 38 38 VAL HB H 2.060 0.003 1 216 38 38 VAL HG1 H 0.860 0.003 1 217 38 38 VAL HG2 H 0.860 0.003 1 218 39 39 ASP H H 8.273 0.001 1 219 39 39 ASP HA H 4.260 0.002 1 220 39 39 ASP HB2 H 2.740 0.003 2 221 39 39 ASP HB3 H 2.600 0.002 2 222 40 40 VAL H H 7.940 1.274 1 223 40 40 VAL HA H 4.090 0.003 1 224 40 40 VAL HB H 2.090 0.003 1 225 40 40 VAL HG1 H 0.870 0.003 1 226 40 40 VAL HG2 H 0.870 0.003 1 227 41 41 MET H H 7.870 0.001 1 228 41 41 MET HA H 4.260 0.003 1 229 41 41 MET HB2 H 1.943 0.003 1 230 41 41 MET HB3 H 1.943 0.003 1 231 41 41 MET HE H 2.040 0.003 1 stop_ save_ save_heteronuclear_noe_list_1 _Saveframe_category heteronuclear_NOE _Details . loop_ _Software_label $XEASY_CARA stop_ loop_ _Experiment_label '2D 1H-15N HSQC' stop_ loop_ _Sample_label . stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 700.13 _Mol_system_component_name entity _Atom_one_atom_name H _Atom_two_atom_name N _Heteronuclear_NOE_value_type 'peak height' _NOE_reference_value 1.5E06 _NOE_reference_description . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Heteronuclear_NOE_value _Heteronuclear_NOE_value_error 3 THR 0.32 . 4 SER 0.42 . 5 HIS 0.46 . 6 LEU 0.34 . 7 LEU 0.57 . 8 ALA 0.53 . 9 LEU 0.56 . 10 LEU 0.52 . 11 LEU 0.54 . 13 LYS 0.37 . 14 SER 0.35 . 16 GLN 0.24 . 17 GLY 0.09 . 18 GLU 0.17 . 19 ASN 0.23 . 20 ARG 0.20 . 21 SER 0.21 . 22 LYS 0.30 . 24 LEU 0.39 . 25 GLY 0.23 . 26 THR 0.27 . 28 TYR 0.43 . 29 ASN 0.49 . 30 PHE 0.40 . 31 SER 0.43 . 32 GLU 0.45 . 33 HIS 0.38 . 34 CYS 0.49 . 35 GLN 0.25 . 36 ASP 0.24 . 37 SER -0.55 . 38 VAL -0.21 . 39 ASP -0.50 . 40 VAL -1.10 . 41 MET -1.85 . stop_ save_ save_heteronuclear_noe_list_2 _Saveframe_category heteronuclear_NOE _Details . loop_ _Software_label $XEASY_CARA stop_ loop_ _Experiment_label '2D 1H-15N HSQC' stop_ loop_ _Sample_label . stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 700.13 _Mol_system_component_name entity _Atom_one_atom_name H _Atom_two_atom_name N _Heteronuclear_NOE_value_type 'peak height' _NOE_reference_value 1.5E06 _NOE_reference_description . _Text_data_format . _Text_data . loop_ _Residue_seq_code _Residue_label _Heteronuclear_NOE_value _Heteronuclear_NOE_value_error 2 ASN 0.55110346 . 3 THR 0.702714064 . 7 LEU 0.641004627 . 8 ALA 0.686119064 . 9 LEU 0.680866232 . 10 LEU 0.664131533 . 11 LEU 0.586177385 . 13 LYS 0.368008375 . 14 SER 0.205424128 . 16 GLN 0.054965497 . 17 GLY -0.041129706 . 18 GLU 0.130451926 . 19 ASN 0.019307614 . 20 ARG -0.023314258 . 21 SER 0.047520225 . 22 LYS 0.120649884 . 24 LEU 0.061152718 . 25 GLY 0.058780438 . 26 THR 0.298746515 . 28 TYR 0.388070124 . 29 ASN 0.42089403 . 30 PHE 0.430495308 . 31 SER 0.45985418 . 32 GLU 0.486145036 . 33 HIS 0.520541339 . 35 GLN 0.550335711 . 36 ASP 0.308163752 . 37 SER 0.277946051 . 38 VAL -0.021194067 . 39 ASP -0.122818028 . 40 VAL -0.396764459 . 41 MET -0.594392716 . stop_ save_