data_18378 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Liraglutide ; _BMRB_accession_number 18378 _BMRB_flat_file_name bmr18378.str _Entry_type original _Submission_date 2012-04-03 _Accession_date 2012-04-03 _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 Ludvigsen Svend . . 2 Steensgaard D. B. . 3 Thomsen J. K. . 4 Strauss H. . . 5 Normann M. . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 162 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2013-07-08 original author . stop_ _Original_release_date 2013-07-08 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'unknown at present' _Citation_status 'in preparation' _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID ? loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Steensgaard D. B. . 2 Thomsen J. K. . 3 Strauss H. . . 4 Normann M. . . 5 Ludvigsen Svend . . stop_ _Journal_abbreviation 'unknown at present' _Journal_name_full 'unknown at present' _Journal_volume . _Journal_issue . _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first . _Page_last . _Year . _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name Liraglutide _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label LIRAGLUTIDE $LIRAGLUTIDE 'N-HEXADECANOYL-L-GLUTAMIC ACID' $entity_D6M stop_ _System_molecular_weight 3751.20 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state 'not present' _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_LIRAGLUTIDE _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common LIRAGLUTIDE _Molecular_mass 3751.20 _Mol_thiol_state 'not present' _Details 'LIRAGLUTIDE IS A HUMAN GLP-1 ANALOG' ############################## # Polymer residue sequence # ############################## _Residue_count 31 _Mol_residue_sequence ; HAEGTFTSDVSSYLEGQAAK EFIAWLVRGRG ; loop_ _Residue_seq_code _Residue_label 1 HIS 2 ALA 3 GLU 4 GLY 5 THR 6 PHE 7 THR 8 SER 9 ASP 10 VAL 11 SER 12 SER 13 TYR 14 LEU 15 GLU 16 GLY 17 GLN 18 ALA 19 ALA 20 LYS 21 GLU 22 PHE 23 ILE 24 ALA 25 TRP 26 LEU 27 VAL 28 ARG 29 GLY 30 ARG 31 GLY stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2014-11-10 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 PDB 4APD Liraglutide 100.00 31 100.00 100.00 1.06e-12 stop_ save_ ############# # Ligands # ############# save_D6M _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common 'N-hexadecanoyl-L-glutamic acid' _BMRB_code D6M _PDB_code D6M _Molecular_mass 385.538 _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 C02 C02 C . 0 . ? C04 C04 C . 0 . ? C05 C05 C . 0 . ? C06 C06 C . 0 . ? C07 C07 C . 0 . ? C09 C09 C . 0 . ? C12 C12 C . 0 . ? C13 C13 C . 0 . ? C14 C14 C . 0 . ? C15 C15 C . 0 . ? C16 C16 C . 0 . ? C17 C17 C . 0 . ? C18 C18 C . 0 . ? C19 C19 C . 0 . ? C20 C20 C . 0 . ? C21 C21 C . 0 . ? C22 C22 C . 0 . ? C23 C23 C . 0 . ? C24 C24 C . 0 . ? C25 C25 C . 0 . ? C26 C26 C . 0 . ? H03 H03 H . 0 . ? H04 H04 H . 0 . ? H051 H051 H . 0 . ? H052 H052 H . 0 . ? H061 H061 H . 0 . ? H062 H062 H . 0 . ? H11 H11 H . 0 . ? H121 H121 H . 0 . ? H122 H122 H . 0 . ? H131 H131 H . 0 . ? H132 H132 H . 0 . ? H141 H141 H . 0 . ? H142 H142 H . 0 . ? H151 H151 H . 0 . ? H152 H152 H . 0 . ? H161 H161 H . 0 . ? H162 H162 H . 0 . ? H171 H171 H . 0 . ? H172 H172 H . 0 . ? H181 H181 H . 0 . ? H182 H182 H . 0 . ? H191 H191 H . 0 . ? H192 H192 H . 0 . ? H201 H201 H . 0 . ? H202 H202 H . 0 . ? H211 H211 H . 0 . ? H212 H212 H . 0 . ? H221 H221 H . 0 . ? H222 H222 H . 0 . ? H231 H231 H . 0 . ? H232 H232 H . 0 . ? H241 H241 H . 0 . ? H242 H242 H . 0 . ? H251 H251 H . 0 . ? H252 H252 H . 0 . ? H261 H261 H . 0 . ? H262 H262 H . 0 . ? H263 H263 H . 0 . ? HX0 HX0 H . 0 . ? N03 N03 N . 0 . ? O01 O01 O . 0 . ? O08 O08 O . 0 . ? O10 O10 O . 0 . ? O11 O11 O . 0 . ? OXT OXT O . 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 O01 C02 ? ? SING C02 N03 ? ? SING C02 C12 ? ? SING N03 C04 ? ? SING C04 C05 ? ? SING C04 C09 ? ? SING C05 C06 ? ? SING C06 C07 ? ? DOUB C07 O08 ? ? SING C07 OXT ? ? DOUB C09 O10 ? ? SING C09 O11 ? ? SING C12 C13 ? ? SING C13 C14 ? ? SING C14 C15 ? ? SING C15 C16 ? ? SING C16 C17 ? ? SING C17 C18 ? ? SING C18 C19 ? ? SING C19 C20 ? ? SING C20 C21 ? ? SING C21 C22 ? ? SING C22 C23 ? ? SING C23 C24 ? ? SING C24 C25 ? ? SING C25 C26 ? ? SING N03 H03 ? ? SING C12 H121 ? ? SING C12 H122 ? ? SING C04 H04 ? ? SING C05 H051 ? ? SING C05 H052 ? ? SING C06 H061 ? ? SING C06 H062 ? ? SING OXT HX0 ? ? SING O11 H11 ? ? SING C13 H131 ? ? SING C13 H132 ? ? SING C14 H141 ? ? SING C14 H142 ? ? SING C15 H151 ? ? SING C15 H152 ? ? SING C16 H161 ? ? SING C16 H162 ? ? SING C17 H171 ? ? SING C17 H172 ? ? SING C18 H181 ? ? SING C18 H182 ? ? SING C19 H191 ? ? SING C19 H192 ? ? SING C20 H201 ? ? SING C20 H202 ? ? SING C21 H211 ? ? SING C21 H212 ? ? SING C22 H221 ? ? SING C22 H222 ? ? SING C23 H231 ? ? SING C23 H232 ? ? SING C24 H241 ? ? SING C24 H242 ? ? SING C25 H251 ? ? SING C25 H252 ? ? SING C26 H261 ? ? SING C26 H262 ? ? SING C26 H263 ? ? 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 $LIRAGLUTIDE 'baker's yeast' 4932 Eukaryota Fungi Saccharomyces cerevisiae 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 _Details $LIRAGLUTIDE 'chemical synthesis' . . . . . 'backbone is produces recombinantly from yeast, and Lysine 26 is subsequently altered with a gammaglu linker and acylated' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '1.6 mmol/l' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $LIRAGLUTIDE 1.6 mM '[U-13C; U-15N]' stop_ save_ ############################ # Computer software used # ############################ save_AutoDep _Saveframe_category software _Name AutoDep _Version 4.3 loop_ _Vendor _Address _Electronic_address AutoDep . . stop_ loop_ _Task collection stop_ _Details . save_ save_CNX _Saveframe_category software _Name CNX _Version any loop_ _Vendor _Address _Electronic_address CNX . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_Pronto _Saveframe_category software _Name Pronto _Version any loop_ _Vendor _Address _Electronic_address 'Kjur, Andersen and Poulsen' . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_XPLOR _Saveframe_category software _Name XPLOR _Version any loop_ _Vendor _Address _Electronic_address Brunger . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_Bruker_AMX-600 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AMX _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name NOESY _Sample_label $sample_1 save_ save_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name TOCSY _Sample_label $sample_1 save_ save_NMR_spectrometer_expt _Saveframe_category NMR_applied_experiment _Experiment_name . _BMRB_pulse_sequence_accession_number . _Details . save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details 'pH [7.9], temp [300], pressure [1], ionStrength [0.0]' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.0 . mM pH 7.900 . pH pressure 1.000 . atm temperature 300.000 . 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 HDO H 1 protons ppm 4.75 internal indirect . . . 1 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_assigned_chem_shift_list _Saveframe_category assigned_chemical_shifts _Details 'Origin nmrStar file /ebi/msd/pdb_root/Processing/prepare/4apd/ebi/liraglutide_nmr_assign_3_4.txt.csh' loop_ _Experiment_label NOESY TOCSY 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 LIRAGLUTIDE _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 HIS HA H 3.97 . 1 2 1 1 HIS HB2 H 3.05 . 2 3 1 1 HIS HB3 H 3.11 . 2 4 1 1 HIS HD2 H 7.05 . 1 5 1 1 HIS HE1 H 7.85 . 1 6 2 2 ALA HA H 4.37 . 1 7 2 2 ALA HB H 1.39 . 1 8 3 3 GLU H H 8.70 . 1 9 3 3 GLU HA H 4.31 . 1 10 3 3 GLU HB2 H 2.00 . 2 11 3 3 GLU HB3 H 2.11 . 2 12 3 3 GLU HG2 H 2.33 . 2 13 3 3 GLU HG3 H 2.33 . 2 14 4 4 GLY H H 8.50 . 1 15 4 4 GLY HA2 H 4.01 . 2 16 4 4 GLY HA3 H 4.01 . 2 17 5 5 THR H H 7.97 . 1 18 5 5 THR HA H 4.34 . 1 19 5 5 THR HB H 4.15 . 1 20 5 5 THR HG2 H 1.11 . 1 21 6 6 PHE H H 8.42 . 1 22 6 6 PHE HA H 4.70 . 1 23 6 6 PHE HB2 H 3.00 . 2 24 6 6 PHE HB3 H 3.13 . 2 25 6 6 PHE HD1 H 7.20 . 3 26 6 6 PHE HD2 H 7.20 . 3 27 6 6 PHE HE1 H 7.25 . 3 28 6 6 PHE HE2 H 7.25 . 3 29 7 7 THR H H 8.12 . 1 30 7 7 THR HA H 4.31 . 1 31 7 7 THR HB H 4.22 . 1 32 7 7 THR HG2 H 1.17 . 1 33 8 8 SER H H 8.24 . 1 34 8 8 SER HA H 4.45 . 1 35 8 8 SER HB2 H 3.93 . 2 36 8 8 SER HB3 H 3.87 . 2 37 9 9 ASP H H 8.43 . 1 38 9 9 ASP HA H 4.68 . 1 39 9 9 ASP HB2 H 2.75 . 2 40 9 9 ASP HB3 H 2.70 . 2 41 10 10 VAL H H 8.17 . 1 42 10 10 VAL HA H 4.05 . 1 43 10 10 VAL HB H 2.11 . 1 44 10 10 VAL HG1 H 0.90 . 2 45 10 10 VAL HG2 H 0.90 . 2 46 11 11 SER H H 8.17 . 1 47 11 11 SER HA H 4.39 . 1 48 11 11 SER HB2 H 3.84 . 2 49 11 11 SER HB3 H 3.84 . 2 50 12 12 SER H H 8.32 . 1 51 12 12 SER HA H 4.30 . 1 52 12 12 SER HB2 H 3.87 . 2 53 12 12 SER HB3 H 3.92 . 2 54 13 13 TYR H H 7.97 . 1 55 13 13 TYR HA H 4.48 . 1 56 13 13 TYR HB2 H 2.95 . 2 57 13 13 TYR HB3 H 3.01 . 2 58 13 13 TYR HD1 H 6.99 . 3 59 13 13 TYR HD2 H 6.99 . 3 60 13 13 TYR HE1 H 6.72 . 3 61 13 13 TYR HE2 H 6.72 . 3 62 14 14 LEU H H 7.96 . 1 63 14 14 LEU HA H 4.18 . 1 64 14 14 LEU HB2 H 1.52 . 2 65 14 14 LEU HB3 H 1.52 . 2 66 14 14 LEU HG H 1.63 . 1 67 14 14 LEU HD1 H 0.79 . 2 68 14 14 LEU HD2 H 0.84 . 2 69 15 15 GLU H H 7.59 . 1 70 15 15 GLU HA H 4.14 . 1 71 15 15 GLU HB2 H 2.16 . 2 72 15 15 GLU HB3 H 1.87 . 2 73 15 15 GLU HG2 H 2.05 . 2 74 15 15 GLU HG3 H 2.05 . 2 75 17 17 GLN H H 8.22 . 1 76 17 17 GLN HA H 4.12 . 1 77 17 17 GLN HB2 H 2.07 . 2 78 17 17 GLN HB3 H 2.07 . 2 79 17 17 GLN HG2 H 2.32 . 2 80 17 17 GLN HG3 H 2.32 . 2 81 17 17 GLN HE21 H 7.53 . 1 82 17 17 GLN HE22 H 6.68 . 1 83 18 18 ALA H H 8.19 . 1 84 18 18 ALA HA H 4.15 . 1 85 18 18 ALA HB H 1.38 . 1 86 19 19 ALA H H 8.07 . 1 87 19 19 ALA HA H 4.03 . 1 88 19 19 ALA HB H 1.36 . 1 89 20 20 LYS HA H 3.89 . 1 90 20 20 LYS HB2 H 1.84 . 2 91 20 20 LYS HG2 H 1.44 . 2 92 20 20 LYS HD2 H 1.36 . 2 93 20 20 LYS HE2 H 3.03 . 2 94 20 20 LYS HZ H 7.74 . 1 95 21 21 GLU H H 8.10 . 1 96 21 21 GLU HA H 4.09 . 1 97 21 21 GLU HB2 H 2.14 . 2 98 21 21 GLU HB3 H 2.09 . 2 99 21 21 GLU HG2 H 2.43 . 2 100 21 21 GLU HG3 H 2.30 . 2 101 22 22 PHE H H 8.07 . 1 102 22 22 PHE HA H 4.30 . 1 103 22 22 PHE HB2 H 3.15 . 2 104 22 22 PHE HB3 H 3.15 . 2 105 22 22 PHE HD1 H 7.01 . 3 106 22 22 PHE HD2 H 7.01 . 3 107 22 22 PHE HE1 H 7.12 . 3 108 22 22 PHE HE2 H 7.12 . 3 109 23 23 ILE H H 8.19 . 1 110 23 23 ILE HA H 3.51 . 1 111 23 23 ILE HB H 1.97 . 1 112 23 23 ILE HG12 H 1.78 . 2 113 23 23 ILE HG13 H 1.25 . 2 114 23 23 ILE HG2 H 0.87 . 1 115 23 23 ILE HD1 H 0.82 . 1 116 24 24 ALA H H 8.03 . 1 117 24 24 ALA HA H 3.96 . 1 118 24 24 ALA HB H 1.48 . 1 119 25 25 TRP H H 7.86 . 1 120 25 25 TRP HA H 4.13 . 1 121 25 25 TRP HB2 H 3.50 . 2 122 25 25 TRP HB3 H 3.25 . 2 123 25 25 TRP HD1 H 7.16 . 1 124 25 25 TRP HE1 H 10.06 . 1 125 25 25 TRP HE3 H 7.22 . 1 126 25 25 TRP HZ2 H 7.36 . 1 127 25 25 TRP HZ3 H 6.84 . 1 128 25 25 TRP HH2 H 7.04 . 1 129 26 26 LEU H H 8.05 . 1 130 26 26 LEU HA H 3.43 . 1 131 26 26 LEU HB2 H 1.64 . 2 132 26 26 LEU HB3 H 1.36 . 2 133 26 26 LEU HG H 1.44 . 1 134 26 26 LEU HD1 H 0.66 . 2 135 26 26 LEU HD2 H 0.66 . 2 136 27 27 VAL H H 7.86 . 1 137 27 27 VAL HA H 3.83 . 1 138 27 27 VAL HB H 2.15 . 1 139 27 27 VAL HG1 H 0.85 . 2 140 27 27 VAL HG2 H 0.90 . 2 141 28 28 ARG H H 7.69 . 1 142 28 28 ARG HA H 4.19 . 1 143 28 28 ARG HB2 H 1.85 . 2 144 28 28 ARG HB3 H 1.85 . 2 145 28 28 ARG HG2 H 1.60 . 2 146 28 28 ARG HG3 H 1.60 . 2 147 28 28 ARG HD2 H 3.07 . 2 148 28 28 ARG HD3 H 3.07 . 2 149 29 29 GLY H H 8.00 . 1 150 29 29 GLY HA2 H 3.77 . 2 151 29 29 GLY HA3 H 3.77 . 2 152 30 30 ARG H H 7.87 . 1 153 30 30 ARG HA H 4.06 . 1 154 30 30 ARG HB2 H 1.62 . 2 155 30 30 ARG HB3 H 1.76 . 2 156 30 30 ARG HG2 H 1.42 . 2 157 30 30 ARG HG3 H 1.34 . 2 158 30 30 ARG HD2 H 2.92 . 2 159 30 30 ARG HD3 H 2.92 . 2 160 31 31 GLY H H 7.82 . 1 161 31 31 GLY HA2 H 3.72 . 2 162 31 31 GLY HA3 H 3.72 . 2 stop_ save_