data_50384 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H and 13C chemical shifts for a mixture of a CB1-derived peptide and a beta-arrestin1-derived peptide in DPC micelles ; _BMRB_accession_number 50384 _BMRB_flat_file_name bmr50384.str _Entry_type original _Submission_date 2020-07-09 _Accession_date 2020-07-09 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details ; CB1-derived peptide encompasses residues 391-409 of CB1 receptor beta-arrestin1-derived peptide encompasses residues 63-76 of beta-arrestin1 ; loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Jimenez 'M. Angeles' . . 2 Morales Paula . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 4 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 250 "13C chemical shifts" 134 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2020-11-18 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 50372 'Free CB1(391-409) peptide in DPC micelles' 50375 'Free beta-arrestin1(63-76) peptide in DPC micelles' 50382 'mixture of a CB1-derived peptide and a beta-arrestin1-derived peptide in aqueous solution' 50383 'mixture of a CB1-derived peptide and a beta-arrestin1-derived peptide in 30% TFE' stop_ _Original_release_date 2020-07-09 save_ ############################# # Citation for this entry # ############################# save_citations_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; Structural Insights into beta-arrestin/CB1 Receptor Interaction: NMR and CD Studies on Model Peptides ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 33143110 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Morales Paula . . 2 Bruix Marta . . 3 Jimenez 'M. Angeles' . . stop_ _Journal_abbreviation 'Int. J. Mol. Sci.' _Journal_name_full 'International journal of molecular sciences' _Journal_volume 21 _Journal_issue 21 _Journal_ISSN 1422-0067 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 8111 _Page_last 8111 _Year 2020 _Details . loop_ _Keyword 'beta arrestin, CB1 receptor, peptide model' stop_ save_ ################################## # Molecular system description # ################################## save_assembly_1 _Saveframe_category molecular_system _Mol_system_name 'barr1(63-76) CB1(391-409)' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label barr1(63-76) $entity_1 CB1(391-409) $entity_2 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 1694.93 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 16 _Mol_residue_sequence ; XYGREDLDVLGLTFRX ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 0 ACE 2 1 TYR 3 2 GLY 4 3 ARG 5 4 GLU 6 5 ASP 7 6 LEU 8 7 ASP 9 8 VAL 10 9 LEU 11 10 GLY 12 11 LEU 13 12 THR 14 13 PHE 15 14 ARG 16 15 NH2 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 2311.74 _Mol_thiol_state 'not present' _Details . _Residue_count 21 _Mol_residue_sequence ; XTVNPIIYALRSKDLRHAFR X ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 0 ACE 2 1 THR 3 2 VAL 4 3 ASN 5 4 PRO 6 5 ILE 7 6 ILE 8 7 TYR 9 8 ALA 10 9 LEU 11 10 ARG 12 11 SER 13 12 LYS 14 13 ASP 15 14 LEU 16 15 ARG 17 16 HIS 18 17 ALA 19 18 PHE 20 19 ARG 21 20 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_ACE _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common 'ACETYL GROUP' _BMRB_code ACE _PDB_code ACE _Standard_residue_derivative . _Molecular_mass 44.053 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C C C . 0 . ? O O O . 0 . ? CH3 CH3 C . 0 . ? H H H . 0 . ? H1 H1 H . 0 . ? H2 H2 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 DOUB C O ? ? SING C CH3 ? ? SING C H ? ? SING CH3 H1 ? ? SING CH3 H2 ? ? SING CH3 H3 ? ? stop_ save_ save_chem_comp_NH2 _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common 'AMINO GROUP' _BMRB_code NH2 _PDB_code NH2 _Standard_residue_derivative . _Molecular_mass 16.023 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? HN1 HN1 H . 0 . ? HN2 HN2 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 N HN1 ? ? SING N HN2 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source_1 _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_1 _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name $entity_1 'chemical synthesis' . . . . . $entity_2 'chemical synthesis' . . . . . 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 _Isotopic_labeling $entity_2 1 mM 'natural abundance' $entity_1 1 mM 'natural abundance' H2O 90 '% v/v' 'natural abundance' D2O 10 '% v/v' [U-2H] DPC 30 mM '[U-98% 2H]' DSS 0.1 mM 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_2 1 mM 'natural abundance' $entity_1 1 mM 'natural abundance' D2O 100 '% v/v' [U-2H] DPC 30 mM '[U-98% 2H]' DSS 0.1 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name TOPSPIN _Version . loop_ _Task collection processing stop_ _Details . save_ save_software_2 _Saveframe_category software _Name NMRFAM-SPARKY _Version . loop_ _Task 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength '600 MHz' _Details . save_ ############################# # NMR applied experiments # ############################# save_1D_1H_1 _Saveframe_category NMR_applied_experiment _Experiment_name '1D 1H' _Sample_label $sample_1 save_ save_2D_1H-1H_COSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H COSY' _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_NOESY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-13C_HSQC_aliphatic_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $sample_1 save_ save_2D_1H-13C_HSQC_aromatic_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aromatic' _Sample_label $sample_1 save_ save_1D_1H_7 _Saveframe_category NMR_applied_experiment _Experiment_name '1D 1H' _Sample_label $sample_2 save_ save_2D_1H-1H_COSY_8 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H COSY' _Sample_label $sample_2 save_ save_2D_1H-1H_TOCSY_9 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_2 save_ save_2D_1H-13C_HSQC_aliphatic_10 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $sample_2 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 5.5 . pH pressure 1 . atm temperature 298 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_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 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_chemical_shifts_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_2 stop_ loop_ _Experiment_label '2D 1H-1H COSY' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '2D 1H-13C HSQC aliphatic' '2D 1H-13C HSQC aromatic' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name barr1(63-76) _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 0 1 ACE H1 H 1.933 0.000 1 2 0 1 ACE H2 H 1.933 0.000 1 3 0 1 ACE H3 H 1.933 0.000 1 4 0 1 ACE CH3 C 24.710 0.000 1 5 1 2 TYR H H 8.147 0.002 1 6 1 2 TYR HA H 4.579 0.003 1 7 1 2 TYR HB2 H 2.800 0.007 2 8 1 2 TYR HB3 H 3.043 0.003 2 9 1 2 TYR HD1 H 7.094 0.005 1 10 1 2 TYR HD2 H 7.094 0.005 1 11 1 2 TYR HE1 H 6.795 0.002 1 12 1 2 TYR HE2 H 6.795 0.002 1 13 1 2 TYR CB C 39.767 0.007 1 14 1 2 TYR CD1 C 133.067 0.000 1 15 1 2 TYR CD2 C 133.067 0.000 1 16 1 2 TYR CE1 C 118.206 0.000 1 17 1 2 TYR CE2 C 118.206 0.000 1 18 2 3 GLY H H 8.810 0.001 1 19 2 3 GLY HA2 H 3.958 0.002 2 20 2 3 GLY HA3 H 4.145 0.004 2 21 3 4 ARG H H 8.560 0.001 1 22 3 4 ARG HA H 4.116 0.004 1 23 3 4 ARG HB2 H 1.841 0.006 2 24 3 4 ARG HB3 H 1.905 0.004 2 25 3 4 ARG HG2 H 1.661 0.005 2 26 3 4 ARG HG3 H 1.661 0.005 2 27 3 4 ARG HD2 H 3.181 0.000 2 28 3 4 ARG HD3 H 3.235 0.002 2 29 3 4 ARG HE H 7.713 0.001 1 30 3 4 ARG CA C 57.908 0.000 1 31 3 4 ARG CB C 30.572 0.003 1 32 3 4 ARG CD C 43.345 0.000 1 33 4 5 GLU H H 9.040 0.002 1 34 4 5 GLU HA H 4.209 0.004 1 35 4 5 GLU HB2 H 1.973 0.004 2 36 4 5 GLU HB3 H 2.065 0.003 2 37 4 5 GLU HG2 H 2.308 0.004 2 38 4 5 GLU HG3 H 2.308 0.004 2 39 4 5 GLU CA C 58.253 0.000 1 40 4 5 GLU CB C 29.322 0.003 1 41 4 5 GLU CG C 36.275 0.000 1 42 5 6 ASP H H 8.110 0.002 1 43 5 6 ASP HA H 4.554 0.000 1 44 5 6 ASP HB2 H 2.707 0.007 2 45 5 6 ASP HB3 H 2.764 0.004 2 46 5 6 ASP CB C 41.105 0.003 1 47 6 7 LEU H H 7.843 0.002 1 48 6 7 LEU HA H 4.202 0.005 1 49 6 7 LEU HB2 H 1.635 0.002 2 50 6 7 LEU HB3 H 1.770 0.003 2 51 6 7 LEU HG H 1.634 0.000 1 52 6 7 LEU HD1 H 0.837 0.003 2 53 6 7 LEU HD2 H 0.914 0.002 2 54 6 7 LEU CB C 42.059 0.006 1 55 6 7 LEU CD1 C 23.848 0.000 1 56 6 7 LEU CD2 C 25.393 0.000 1 57 7 8 ASP H H 8.152 0.003 1 58 7 8 ASP HA H 4.560 0.001 1 59 7 8 ASP HB2 H 2.716 0.003 2 60 7 8 ASP HB3 H 2.716 0.003 2 61 7 8 ASP CB C 40.563 0.000 1 62 8 9 VAL H H 7.921 0.001 1 63 8 9 VAL HA H 3.957 0.004 1 64 8 9 VAL HB H 2.213 0.003 1 65 8 9 VAL HG1 H 0.974 0.004 2 66 8 9 VAL HG2 H 1.034 0.005 2 67 8 9 VAL CA C 64.210 0.000 1 68 8 9 VAL CB C 32.144 0.000 1 69 8 9 VAL CG1 C 21.290 0.000 1 70 8 9 VAL CG2 C 21.388 0.000 1 71 9 10 LEU H H 7.984 0.002 1 72 9 10 LEU HA H 4.183 0.000 1 73 9 10 LEU HB2 H 1.613 0.002 2 74 9 10 LEU HB3 H 1.859 0.000 2 75 9 10 LEU HD1 H 0.859 0.000 2 76 9 10 LEU HD2 H 0.917 0.000 2 77 9 10 LEU CA C 56.294 0.000 1 78 9 10 LEU CB C 41.905 0.013 1 79 9 10 LEU CD1 C 23.637 0.000 1 80 9 10 LEU CD2 C 25.455 0.000 1 81 10 11 GLY H H 8.107 0.001 1 82 10 11 GLY HA2 H 3.837 0.001 2 83 10 11 GLY HA3 H 3.958 0.001 2 84 11 12 LEU H H 7.942 0.001 1 85 11 12 LEU HA H 4.256 0.001 1 86 11 12 LEU HB2 H 1.502 0.004 2 87 11 12 LEU HB3 H 1.739 0.000 2 88 11 12 LEU HG H 1.745 0.000 1 89 11 12 LEU HD1 H 0.873 0.000 2 90 11 12 LEU HD2 H 0.931 0.000 2 91 11 12 LEU CB C 42.451 0.033 1 92 11 12 LEU CD1 C 23.508 0.000 1 93 11 12 LEU CD2 C 25.516 0.000 1 94 12 13 THR H H 7.992 0.003 1 95 12 13 THR HA H 4.210 0.004 1 96 12 13 THR HB H 4.085 0.006 1 97 12 13 THR HG2 H 1.053 0.002 1 98 12 13 THR CA C 62.971 0.000 1 99 12 13 THR CB C 69.863 0.000 1 100 12 13 THR CG2 C 21.455 0.000 1 101 13 14 PHE H H 8.190 0.002 1 102 13 14 PHE HA H 4.583 0.005 1 103 13 14 PHE HB2 H 3.020 0.004 2 104 13 14 PHE HB3 H 3.162 0.005 2 105 13 14 PHE HD1 H 7.266 0.002 1 106 13 14 PHE HD2 H 7.266 0.002 1 107 13 14 PHE HE1 H 7.267 0.000 1 108 13 14 PHE HE2 H 7.267 0.000 1 109 13 14 PHE HZ H 7.175 0.000 1 110 13 14 PHE CB C 39.724 0.006 1 111 13 14 PHE CD1 C 132.020 0.000 1 112 13 14 PHE CD2 C 132.020 0.000 1 113 13 14 PHE CE1 C 131.223 0.000 1 114 13 14 PHE CE2 C 131.223 0.000 1 115 13 14 PHE CZ C 129.437 0.000 1 116 14 15 ARG H H 8.141 0.004 1 117 14 15 ARG HA H 4.232 0.002 1 118 14 15 ARG HB2 H 1.734 0.002 2 119 14 15 ARG HB3 H 1.867 0.002 2 120 14 15 ARG HG2 H 1.577 0.006 2 121 14 15 ARG HG3 H 1.627 0.008 2 122 14 15 ARG HD2 H 3.165 0.004 2 123 14 15 ARG HD3 H 3.165 0.004 2 124 14 15 ARG HE H 7.408 0.003 1 125 14 15 ARG CB C 30.964 0.007 1 126 14 15 ARG CD C 43.473 0.000 1 127 15 16 NH2 HN1 H 7.129 0.002 2 128 15 16 NH2 HN2 H 7.256 0.000 2 stop_ save_ save_assigned_chemical_shifts_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_2 stop_ loop_ _Experiment_label '2D 1H-1H COSY' '2D 1H-1H TOCSY' '2D 1H-13C HSQC aliphatic' stop_ loop_ _Sample_label $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name barr1(63-76) _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 2 TYR HA H 4.576 0.000 1 2 1 2 TYR CA C 58.422 0.000 1 3 3 4 ARG HA H 4.083 0.000 1 4 3 4 ARG CA C 57.979 0.000 1 5 4 5 GLU HA H 4.235 0.000 1 6 4 5 GLU CA C 57.948 0.000 1 7 5 6 ASP HA H 4.551 0.000 1 8 5 6 ASP CA C 55.560 0.000 1 9 6 7 LEU HA H 4.223 0.000 1 10 6 7 LEU CA C 55.712 0.000 1 11 7 8 ASP HA H 4.580 0.000 1 12 7 8 ASP CA C 55.350 0.000 1 13 8 9 VAL HA H 3.963 0.000 1 14 8 9 VAL CA C 64.229 0.000 1 15 9 10 LEU HA H 4.182 0.000 1 16 9 10 LEU CA C 56.342 0.000 1 17 11 12 LEU HA H 4.273 0.000 1 18 11 12 LEU CA C 55.604 0.000 1 19 12 13 THR HA H 4.222 0.003 1 20 12 13 THR HB H 4.080 0.000 1 21 12 13 THR CA C 62.958 0.000 1 22 12 13 THR CB C 69.744 0.000 1 23 13 14 PHE HA H 4.591 0.000 1 24 13 14 PHE CA C 58.107 0.000 1 25 14 15 ARG HA H 4.244 0.000 1 26 14 15 ARG CA C 56.049 0.000 1 stop_ save_ save_assigned_chemical_shifts_3 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_2 stop_ loop_ _Experiment_label '2D 1H-1H COSY' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '2D 1H-13C HSQC aliphatic' '2D 1H-13C HSQC aromatic' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name CB1(391-409) _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 0 1 ACE H1 H 2.077 0.001 1 2 0 1 ACE H2 H 2.077 0.001 1 3 0 1 ACE H3 H 2.077 0.001 1 4 0 1 ACE CH3 C 24.720 0.000 1 5 1 2 THR H H 8.278 0.001 1 6 1 2 THR HA H 4.263 0.004 1 7 1 2 THR HB H 4.111 0.004 1 8 1 2 THR HG2 H 1.190 0.001 1 9 1 2 THR CA C 62.816 0.000 1 10 1 2 THR CB C 69.926 0.000 1 11 1 2 THR CG2 C 21.856 0.000 1 12 2 3 VAL H H 8.236 0.002 1 13 2 3 VAL HA H 4.124 0.006 1 14 2 3 VAL HB H 2.084 0.001 1 15 2 3 VAL HG1 H 0.910 0.008 2 16 2 3 VAL HG2 H 0.942 0.006 2 17 2 3 VAL CA C 62.206 0.000 1 18 2 3 VAL CB C 33.005 0.000 1 19 2 3 VAL CG1 C 21.296 0.000 1 20 2 3 VAL CG2 C 20.921 0.000 1 21 3 4 ASN H H 8.655 0.003 1 22 3 4 ASN HB2 H 2.941 0.001 2 23 3 4 ASN HB3 H 2.702 0.000 2 24 3 4 ASN HD21 H 6.732 0.001 2 25 3 4 ASN HD22 H 8.109 0.003 2 26 4 5 PRO HA H 4.356 0.004 1 27 4 5 PRO HB2 H 1.884 0.000 2 28 4 5 PRO HB3 H 2.419 0.004 2 29 4 5 PRO HG2 H 2.064 0.004 2 30 4 5 PRO HG3 H 2.064 0.004 2 31 4 5 PRO HD2 H 3.747 0.001 2 32 4 5 PRO HD3 H 3.862 0.007 2 33 4 5 PRO CB C 32.344 0.016 1 34 4 5 PRO CG C 27.848 0.000 1 35 4 5 PRO CD C 50.939 0.005 1 36 5 6 ILE H H 8.015 0.003 1 37 5 6 ILE HA H 3.823 0.004 1 38 5 6 ILE HB H 2.020 0.000 1 39 5 6 ILE HG12 H 1.189 0.010 2 40 5 6 ILE HG13 H 1.668 0.000 2 41 5 6 ILE HG2 H 0.875 0.000 1 42 5 6 ILE HD1 H 0.911 0.000 1 43 5 6 ILE CA C 64.387 0.000 1 44 5 6 ILE CB C 37.614 0.000 1 45 5 6 ILE CG1 C 29.136 0.000 1 46 5 6 ILE CG2 C 17.651 0.000 1 47 5 6 ILE CD1 C 13.325 0.000 1 48 6 7 ILE H H 7.601 0.001 1 49 6 7 ILE HA H 3.671 0.003 1 50 6 7 ILE HB H 1.993 0.008 1 51 6 7 ILE HG12 H 1.218 0.004 2 52 6 7 ILE HG13 H 1.555 0.006 2 53 6 7 ILE HG2 H 0.872 0.004 1 54 6 7 ILE HD1 H 0.854 0.000 1 55 6 7 ILE CA C 64.098 0.000 1 56 6 7 ILE CB C 37.131 0.000 1 57 6 7 ILE CG1 C 28.562 0.003 1 58 6 7 ILE CG2 C 17.651 0.000 1 59 6 7 ILE CD1 C 12.270 0.000 1 60 7 8 TYR H H 8.096 0.004 1 61 7 8 TYR HA H 4.111 0.004 1 62 7 8 TYR HB2 H 3.025 0.003 2 63 7 8 TYR HB3 H 3.066 0.002 2 64 7 8 TYR HD1 H 7.085 0.004 1 65 7 8 TYR HD2 H 7.085 0.004 1 66 7 8 TYR HE1 H 6.808 0.005 1 67 7 8 TYR HE2 H 6.808 0.005 1 68 7 8 TYR CA C 61.024 0.000 1 69 7 8 TYR CB C 38.125 0.012 1 70 7 8 TYR CD1 C 132.929 0.000 1 71 7 8 TYR CD2 C 132.929 0.000 1 72 7 8 TYR CE1 C 118.320 0.000 1 73 7 8 TYR CE2 C 118.320 0.000 1 74 8 9 ALA H H 7.900 0.002 1 75 8 9 ALA HA H 4.075 0.004 1 76 8 9 ALA HB H 1.543 0.003 1 77 8 9 ALA CA C 54.783 0.000 1 78 8 9 ALA CB C 18.641 0.000 1 79 9 10 LEU H H 7.949 0.003 1 80 9 10 LEU HA H 4.079 0.003 1 81 9 10 LEU HB2 H 1.538 0.007 2 82 9 10 LEU HB3 H 1.906 0.011 2 83 9 10 LEU HG H 1.921 0.000 1 84 9 10 LEU HD1 H 0.851 0.007 2 85 9 10 LEU HD2 H 0.874 0.001 2 86 9 10 LEU CA C 57.148 0.000 1 87 9 10 LEU CB C 42.181 0.006 1 88 9 10 LEU CG C 26.948 0.000 1 89 9 10 LEU CD1 C 23.530 0.000 1 90 9 10 LEU CD2 C 25.831 0.000 1 91 10 11 ARG H H 7.948 0.003 1 92 10 11 ARG HA H 4.179 0.003 1 93 10 11 ARG HB2 H 1.806 0.003 2 94 10 11 ARG HB3 H 1.905 0.009 2 95 10 11 ARG HG2 H 1.671 0.003 2 96 10 11 ARG HD2 H 3.088 0.004 2 97 10 11 ARG HD3 H 3.088 0.004 2 98 10 11 ARG HE H 7.460 0.000 1 99 10 11 ARG CD C 43.808 0.000 1 100 11 12 SER H H 7.763 0.002 1 101 11 12 SER HA H 4.321 0.002 1 102 11 12 SER HB2 H 3.795 0.001 2 103 11 12 SER HB3 H 3.867 0.005 2 104 12 13 LYS H H 7.981 0.003 1 105 12 13 LYS HA H 4.245 0.006 1 106 12 13 LYS HB2 H 1.784 0.004 2 107 12 13 LYS HB3 H 1.864 0.005 2 108 12 13 LYS HG2 H 1.442 0.000 2 109 12 13 LYS HG3 H 1.471 0.000 2 110 12 13 LYS HD2 H 1.658 0.000 2 111 12 13 LYS HD3 H 1.658 0.000 2 112 12 13 LYS HE2 H 2.922 0.000 2 113 12 13 LYS HE3 H 2.922 0.000 2 114 12 13 LYS CB C 32.801 0.009 1 115 12 13 LYS CG C 24.852 0.002 1 116 12 13 LYS CD C 28.906 0.000 1 117 12 13 LYS CE C 42.114 0.000 1 118 13 14 ASP H H 8.308 0.002 1 119 13 14 ASP HA H 4.660 0.000 1 120 13 14 ASP HB2 H 2.551 0.007 2 121 13 14 ASP HB3 H 2.837 0.004 2 122 13 14 ASP CB C 40.538 0.015 1 123 14 15 LEU H H 8.354 0.001 1 124 14 15 LEU HA H 4.084 0.004 1 125 14 15 LEU HB2 H 1.601 0.008 2 126 14 15 LEU HB3 H 1.767 0.004 2 127 14 15 LEU HG H 1.762 0.000 1 128 14 15 LEU HD1 H 0.869 0.002 2 129 14 15 LEU HD2 H 0.962 0.004 2 130 14 15 LEU CA C 57.148 0.000 1 131 14 15 LEU CB C 42.097 0.013 1 132 14 15 LEU CG C 27.240 0.000 1 133 14 15 LEU CD1 C 23.937 0.000 1 134 14 15 LEU CD2 C 25.515 0.000 1 135 15 16 ARG H H 8.280 0.001 1 136 15 16 ARG HA H 3.965 0.004 1 137 15 16 ARG HB2 H 1.772 0.002 2 138 15 16 ARG HB3 H 1.804 0.000 2 139 15 16 ARG HG2 H 1.517 0.007 2 140 15 16 ARG HG3 H 1.562 0.001 2 141 15 16 ARG HD2 H 3.182 0.003 2 142 15 16 ARG HD3 H 3.182 0.003 2 143 15 16 ARG HE H 7.709 0.002 1 144 15 16 ARG CA C 58.929 0.000 1 145 15 16 ARG CB C 29.901 0.010 1 146 15 16 ARG CG C 27.894 0.006 1 147 15 16 ARG CD C 43.432 0.000 1 148 16 17 HIS H H 7.875 0.004 1 149 16 17 HIS HA H 4.541 0.006 1 150 16 17 HIS HB2 H 3.107 0.005 2 151 16 17 HIS HB3 H 3.311 0.003 2 152 16 17 HIS HD2 H 7.215 0.004 1 153 16 17 HIS HE1 H 8.325 0.006 1 154 16 17 HIS CB C 29.182 0.000 1 155 16 17 HIS CD2 C 119.793 0.000 1 156 16 17 HIS CE1 C 136.839 0.000 1 157 17 18 ALA H H 7.785 0.001 1 158 17 18 ALA HA H 4.079 0.004 1 159 17 18 ALA HB H 1.263 0.004 1 160 17 18 ALA CA C 54.053 0.000 1 161 17 18 ALA CB C 18.883 0.000 1 162 18 19 PHE H H 7.881 0.005 1 163 18 19 PHE HA H 4.510 0.004 1 164 18 19 PHE HB2 H 3.017 0.005 2 165 18 19 PHE HB3 H 3.234 0.004 2 166 18 19 PHE HD1 H 7.285 0.005 1 167 18 19 PHE HD2 H 7.285 0.005 1 168 18 19 PHE HE1 H 7.227 0.000 1 169 18 19 PHE HE2 H 7.227 0.000 1 170 18 19 PHE HZ H 7.124 0.000 1 171 18 19 PHE CB C 39.535 0.017 1 172 18 19 PHE CD1 C 132.049 0.000 1 173 18 19 PHE CD2 C 132.049 0.000 1 174 18 19 PHE CE1 C 130.974 0.000 1 175 18 19 PHE CE2 C 130.974 0.000 1 176 18 19 PHE CZ C 129.121 0.000 1 177 19 20 ARG H H 7.872 0.002 1 178 19 20 ARG HA H 4.231 0.003 1 179 19 20 ARG HB2 H 1.785 0.006 2 180 19 20 ARG HB3 H 1.897 0.005 2 181 19 20 ARG HG2 H 1.621 0.002 2 182 19 20 ARG HG3 H 1.656 0.005 2 183 19 20 ARG HD2 H 3.162 0.005 2 184 19 20 ARG HD3 H 3.162 0.005 2 185 19 20 ARG HE H 7.452 0.003 1 186 19 20 ARG CB C 30.886 0.020 1 187 19 20 ARG CD C 43.511 0.000 1 188 20 21 NH2 HN1 H 7.195 0.001 2 189 20 21 NH2 HN2 H 7.396 0.001 2 stop_ save_ save_assigned_chemical_shifts_4 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_2 stop_ loop_ _Experiment_label '2D 1H-1H COSY' '2D 1H-1H TOCSY' '2D 1H-13C HSQC aliphatic' stop_ loop_ _Sample_label $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name CB1(391-409) _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 2 THR HA H 4.266 0.000 1 2 1 2 THR HB H 4.110 0.000 1 3 1 2 THR CA C 62.816 0.000 1 4 1 2 THR CB C 69.831 0.000 1 5 2 3 VAL HA H 4.126 0.000 1 6 2 3 VAL CA C 62.127 0.000 1 7 4 5 PRO HA H 4.368 0.000 1 8 4 5 PRO CA C 65.371 0.000 1 9 5 6 ILE HA H 3.821 0.000 1 10 5 6 ILE CA C 64.387 0.000 1 11 6 7 ILE HA H 3.668 0.000 1 12 6 7 ILE CA C 64.124 0.000 1 13 7 8 TYR HA H 4.124 0.000 1 14 7 8 TYR CA C 60.955 0.000 1 15 8 9 ALA HA H 4.073 0.000 1 16 8 9 ALA CA C 54.718 0.000 1 17 9 10 LEU HA H 4.076 0.000 1 18 9 10 LEU CA C 57.125 0.000 1 19 10 11 ARG HA H 4.174 0.000 1 20 10 11 ARG CA C 57.663 0.000 1 21 11 12 SER HA H 4.334 0.000 1 22 11 12 SER HB2 H 3.794 0.000 2 23 11 12 SER HB3 H 3.864 0.000 2 24 11 12 SER CA C 59.309 0.000 1 25 11 12 SER CB C 63.835 0.022 1 26 12 13 LYS HA H 4.261 0.000 1 27 12 13 LYS CA C 56.310 0.000 1 28 13 14 ASP HA H 4.679 0.001 1 29 13 14 ASP CA C 53.814 0.000 1 30 14 15 LEU HA H 4.076 0.000 1 31 14 15 LEU CA C 57.125 0.000 1 32 15 16 ARG HA H 3.965 0.000 1 33 15 16 ARG CA C 58.811 0.000 1 34 16 17 HIS HA H 4.588 0.000 1 35 16 17 HIS CA C 56.626 0.000 1 36 17 18 ALA HA H 4.086 0.000 1 37 17 18 ALA CA C 53.964 0.000 1 38 18 19 PHE HA H 4.518 0.000 1 39 18 19 PHE CA C 58.139 0.000 1 40 19 20 ARG HA H 4.244 0.000 1 41 19 20 ARG CA C 56.049 0.000 1 stop_ save_