data_19071 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; SOLUTION STRUCTURE OF LIPIDATED GLUCAGON ANALOG IN D-TFE ; _BMRB_accession_number 19071 _BMRB_flat_file_name bmr19071.str _Entry_type original _Submission_date 2013-03-03 _Accession_date 2013-03-03 _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 Ward B. P. . 2 Ma D. . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 4 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 172 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2014-02-14 update BMRB 'update entry citation' 2013-04-03 update author 'update entry citation' 2013-03-25 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 19070 'GLUCAGON AIB2,16 LYS13-GAMMAGLU-GAMMAGLU-C16 AMIDE (IN WATER)' stop_ save_ ############################# # Citation for this entry # ############################# save_citations _Saveframe_category entry_citation _Citation_full . _Citation_title 'Peptide lipidation stabilizes structure to enhance biological function.' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 24327962 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Ward Brian P. . 2 Ottaway Nickki L. . 3 Perez-Tilve Diego . . 4 Ma Dejian . . 5 Gelfanov Vasily M. . 6 Tschop Matthias H. . 7 Dimarchi Richard D. . stop_ _Journal_abbreviation 'Mol Metab' _Journal_name_full 'Molecular metabolism' _Journal_volume 2 _Journal_issue 4 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 468 _Page_last 479 _Year 2013 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'GLUCAGON AIB2,16 LYS13-GAMMAGLU-GAMMAGLU-C16 AMIDE' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'GLUCAGON AIB2,16 LYS13-GAMMAGLU-GAMMAGLU-C16 AMIDE' $GLUCAGON_AIB2-16_LYS13-GAMMAGLU-GAMMAGLU-C16_AMIDE 'GGL, 1' $entity_GGL 'GGL, 2' $entity_GGL PLM $entity_PLM 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_GLUCAGON_AIB2-16_LYS13-GAMMAGLU-GAMMAGLU-C16_AMIDE _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common GLUCAGON_AIB2-16_LYS13-GAMMAGLU-GAMMAGLU-C16_AMIDE _Molecular_mass 4269.445 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 30 _Mol_residue_sequence ; HXQGTFTSDYSKKLDXRRAQ DFVQWLMNTX ; loop_ _Residue_seq_code _Residue_label 1 HIS 2 AIB 3 GLN 4 GLY 5 THR 6 PHE 7 THR 8 SER 9 ASP 10 TYR 11 SER 12 LYS 13 LYS 14 LEU 15 ASP 16 AIB 17 ARG 18 ARG 19 ALA 20 GLN 21 ASP 22 PHE 23 VAL 24 GLN 25 TRP 26 LEU 27 MET 28 ASN 29 THR 30 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2014-11-09 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 19070 GLUCAGON_AIB2-16_LYS13-GAMMAGLU-GAMMAGLU-C16_AMIDE 96.67 30 100.00 100.00 4.48e-10 PDB 2M5P "Solution Structure Of Lipidated Glucagon Analog In Water" 96.67 30 100.00 100.00 4.48e-10 PDB 2M5Q "Solution Structure Of Lipidated Glucagon Analog In D-tfe" 96.67 30 100.00 100.00 4.48e-10 stop_ save_ ###################### # Polymer residues # ###################### save_chem_comp_AIB _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common 'ALPHA-AMINOISOBUTYRIC ACID' _BMRB_code AIB _PDB_code AIB _Standard_residue_derivative . _Molecular_mass 103.120 _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 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? CB1 CB1 C . 0 . ? CB2 CB2 C . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HO2 HO2 H . 0 . ? HB11 HB11 H . 0 . ? HB12 HB12 H . 0 . ? HB13 HB13 H . 0 . ? HB21 HB21 H . 0 . ? HB22 HB22 H . 0 . ? HB23 HB23 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 CA ? ? SING N H ? ? SING N H2 ? ? SING CA C ? ? SING CA CB1 ? ? SING CA CB2 ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HO2 ? ? SING CB1 HB11 ? ? SING CB1 HB12 ? ? SING CB1 HB13 ? ? SING CB2 HB21 ? ? SING CB2 HB22 ? ? SING CB2 HB23 ? ? 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_ ############# # Ligands # ############# save_GGL _Saveframe_category ligand _Mol_type "non-polymer (L-GAMMA-PEPTIDE, C-DELTA LINKING)" _Name_common "entity_GGL (GAMMA-L-GLUTAMIC ACID)" _BMRB_code GGL _PDB_code GGL _Molecular_mass 147.129 _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 N N N . 0 . ? CA CA C . 0 . ? C C C . 0 . ? O O O . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD CD C . 0 . ? OE1 OE1 O . 0 . ? OE2 OE2 O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 H . 0 . ? HE2 HE2 H . 0 . ? HXT HXT 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 CA ? ? SING N H ? ? SING N H2 ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING C OXT ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD ? ? SING CG HG2 ? ? SING CG HG3 ? ? DOUB CD OE1 ? ? SING CD OE2 ? ? SING OE2 HE2 ? ? SING OXT HXT ? ? stop_ _Mol_thiol_state . _Sequence_homology_query_date . save_ save_PLM _Saveframe_category ligand _Mol_type "non-polymer (NON-POLYMER)" _Name_common "entity_PLM (PALMITIC ACID)" _BMRB_code PLM _PDB_code PLM _Molecular_mass 256.424 _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 C1 C1 C . 0 . ? O1 O1 O . 0 . ? O2 O2 O . 0 . ? C2 C2 C . 0 . ? C3 C3 C . 0 . ? C4 C4 C . 0 . ? C5 C5 C . 0 . ? C6 C6 C . 0 . ? C7 C7 C . 0 . ? C8 C8 C . 0 . ? C9 C9 C . 0 . ? CA CA C . 0 . ? CB CB C . 0 . ? CC CC C . 0 . ? CD CD C . 0 . ? CE CE C . 0 . ? CF CF C . 0 . ? CG CG C . 0 . ? H H H . 0 . ? H21 H21 H . 0 . ? H22 H22 H . 0 . ? H31 H31 H . 0 . ? H32 H32 H . 0 . ? H41 H41 H . 0 . ? H42 H42 H . 0 . ? H51 H51 H . 0 . ? H52 H52 H . 0 . ? H61 H61 H . 0 . ? H62 H62 H . 0 . ? H71 H71 H . 0 . ? H72 H72 H . 0 . ? H81 H81 H . 0 . ? H82 H82 H . 0 . ? H91 H91 H . 0 . ? H92 H92 H . 0 . ? HA1 HA1 H . 0 . ? HA2 HA2 H . 0 . ? HB1 HB1 H . 0 . ? HB2 HB2 H . 0 . ? HC1 HC1 H . 0 . ? HC2 HC2 H . 0 . ? HD1 HD1 H . 0 . ? HD2 HD2 H . 0 . ? HE1 HE1 H . 0 . ? HE2 HE2 H . 0 . ? HF1 HF1 H . 0 . ? HF2 HF2 H . 0 . ? HG1 HG1 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 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 C1 O1 ? ? DOUB C1 O2 ? ? SING C1 C2 ? ? SING O1 H ? ? SING C2 C3 ? ? SING C2 H21 ? ? SING C2 H22 ? ? SING C3 C4 ? ? SING C3 H31 ? ? SING C3 H32 ? ? SING C4 C5 ? ? SING C4 H41 ? ? SING C4 H42 ? ? SING C5 C6 ? ? SING C5 H51 ? ? SING C5 H52 ? ? SING C6 C7 ? ? SING C6 H61 ? ? SING C6 H62 ? ? SING C7 C8 ? ? SING C7 H71 ? ? SING C7 H72 ? ? SING C8 C9 ? ? SING C8 H81 ? ? SING C8 H82 ? ? SING C9 CA ? ? SING C9 H91 ? ? SING C9 H92 ? ? SING CA CB ? ? SING CA HA1 ? ? SING CA HA2 ? ? SING CB CC ? ? SING CB HB1 ? ? SING CB HB2 ? ? SING CC CD ? ? SING CC HC1 ? ? SING CC HC2 ? ? SING CD CE ? ? SING CD HD1 ? ? SING CD HD2 ? ? SING CE CF ? ? SING CE HE1 ? ? SING CE HE2 ? ? SING CF CG ? ? SING CF HF1 ? ? SING CF HF2 ? ? SING CG HG1 ? ? SING CG HG2 ? ? SING CG HG3 ? ? 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 $GLUCAGON_AIB2-16_LYS13-GAMMAGLU-GAMMAGLU-C16_AMIDE . . . . . . 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 $GLUCAGON_AIB2-16_LYS13-GAMMAGLU-GAMMAGLU-C16_AMIDE 'chemical synthesis' . . . . . 'SEQUENCE ORIGINATES FROM A NATURAL HUMAN SEQ' 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 $GLUCAGON_AIB2-16_LYS13-GAMMAGLU-GAMMAGLU-C16_AMIDE 0.7 mM 'natural abundance' 'sodium phosphate' 20 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_XPLOR-NIH _Saveframe_category software _Name 'X-PLOR NIH' _Version . loop_ _Vendor _Address _Electronic_address BRUNGER . . stop_ loop_ _Task refinement stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model 'Uniform NMR System' _Field_strength 800 _Details 'Not sure what the model is...' 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-1H_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _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 . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.02 . M pH 4.7 . pH pressure 1 . atm temperature 298 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference_1 _Saveframe_category chemical_shift_reference _Details 'Used the deuterium proton signal as reference' 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 water H 1 protons ppm 4.65 internal direct . . . 1.0 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-1H TOCSY' '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 'GLUCAGON AIB2,16 LYS13-GAMMAGLU-GAMMAGLU-C16 AMIDE' _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 HB2 H 3.279 0.004 2 2 1 1 HIS HB3 H 3.388 0.004 2 3 1 1 HIS HD2 H 7.195 0.002 1 4 1 1 HIS HE1 H 7.745 0.000 1 5 1 1 HIS HE2 H 8.206 0.006 1 6 2 2 AIB HB11 H 1.313 0.005 1 7 2 2 AIB HB12 H 1.313 0.005 1 8 2 2 AIB HB13 H 1.313 0.005 1 9 2 2 AIB HB21 H 1.406 0.000 1 10 2 2 AIB HB22 H 1.406 0.000 1 11 2 2 AIB HB23 H 1.406 0.000 1 12 3 3 GLN HA H 3.978 0.005 1 13 3 3 GLN HB2 H 1.940 0.051 2 14 3 3 GLN HB3 H 2.045 0.008 2 15 3 3 GLN HG2 H 2.362 0.004 2 16 3 3 GLN HG3 H 2.536 0.004 2 17 4 4 GLY HA2 H 3.943 0.002 2 18 4 4 GLY HA3 H 4.083 0.001 2 19 5 5 THR HA H 4.088 0.003 1 20 5 5 THR HB H 3.874 0.004 1 21 5 5 THR HG2 H 1.133 0.003 1 22 6 6 PHE HA H 4.292 0.005 1 23 6 6 PHE HB2 H 3.095 0.009 2 24 6 6 PHE HB3 H 3.110 0.007 2 25 6 6 PHE HD1 H 7.063 0.047 1 26 6 6 PHE HD2 H 7.063 0.047 1 27 6 6 PHE HE1 H 7.106 0.011 1 28 6 6 PHE HE2 H 7.106 0.011 1 29 7 7 THR HA H 4.234 0.004 1 30 7 7 THR HB H 3.908 0.004 1 31 7 7 THR HG2 H 1.284 0.004 1 32 8 8 SER HA H 4.081 0.002 1 33 8 8 SER HB2 H 3.941 0.008 2 34 8 8 SER HB3 H 3.941 0.008 2 35 9 9 ASP HA H 4.439 0.005 1 36 9 9 ASP HB2 H 2.773 0.007 2 37 9 9 ASP HB3 H 2.968 0.006 2 38 10 10 TYR HA H 4.118 0.003 1 39 10 10 TYR HB2 H 2.810 0.002 2 40 10 10 TYR HB3 H 2.828 0.002 2 41 10 10 TYR HD1 H 6.889 0.069 1 42 10 10 TYR HD2 H 6.889 0.069 1 43 10 10 TYR HE1 H 6.716 0.091 1 44 10 10 TYR HE2 H 6.716 0.091 1 45 11 11 SER HA H 4.083 0.002 1 46 11 11 SER HB2 H 3.972 0.010 2 47 11 11 SER HB3 H 3.972 0.010 2 48 12 12 LYS HA H 4.041 0.008 1 49 12 12 LYS HB2 H 1.656 0.000 2 50 12 12 LYS HB3 H 1.726 0.004 2 51 12 12 LYS HG2 H 1.391 0.004 2 52 12 12 LYS HG3 H 1.391 0.004 2 53 12 12 LYS HD2 H 1.648 0.014 2 54 12 12 LYS HD3 H 1.853 0.003 2 55 12 12 LYS HE2 H 2.889 0.004 2 56 12 12 LYS HE3 H 2.958 0.005 2 57 13 13 LYS H H 7.585 0.000 1 58 13 13 LYS HA H 3.881 0.002 1 59 13 13 LYS HB2 H 1.748 0.012 2 60 13 13 LYS HB3 H 1.780 0.010 2 61 13 13 LYS HG2 H 1.373 0.013 2 62 13 13 LYS HG3 H 1.439 0.007 2 63 13 13 LYS HD2 H 1.478 0.000 2 64 13 13 LYS HD3 H 1.565 0.004 2 65 13 13 LYS HE2 H 3.084 0.006 2 66 13 13 LYS HE3 H 3.115 0.003 2 67 14 14 LEU HA H 3.938 0.006 1 68 14 14 LEU HB2 H 1.404 0.026 2 69 14 14 LEU HB3 H 1.467 0.008 2 70 14 14 LEU HG H 1.608 0.049 1 71 14 14 LEU HD1 H 0.736 0.008 1 72 14 14 LEU HD2 H 0.736 0.008 1 73 15 15 ASP HA H 4.245 0.006 1 74 15 15 ASP HB2 H 2.740 0.011 2 75 15 15 ASP HB3 H 3.049 0.014 2 76 16 16 AIB HB11 H 1.434 0.056 1 77 16 16 AIB HB12 H 1.434 0.056 1 78 16 16 AIB HB13 H 1.434 0.056 1 79 16 16 AIB HB21 H 1.493 0.003 1 80 16 16 AIB HB22 H 1.493 0.003 1 81 16 16 AIB HB23 H 1.493 0.003 1 82 17 17 ARG H H 7.930 0.002 1 83 17 17 ARG HA H 3.985 0.014 1 84 17 17 ARG HB2 H 1.857 0.021 2 85 17 17 ARG HB3 H 1.968 0.015 2 86 17 17 ARG HG2 H 1.565 0.003 2 87 17 17 ARG HG3 H 1.638 0.000 2 88 17 17 ARG HD2 H 3.065 0.002 2 89 17 17 ARG HD3 H 3.101 0.014 2 90 18 18 ARG H H 7.925 0.007 1 91 18 18 ARG HA H 3.998 0.010 1 92 18 18 ARG HB2 H 1.740 0.007 2 93 18 18 ARG HB3 H 1.926 0.012 2 94 18 18 ARG HG2 H 1.580 0.002 2 95 18 18 ARG HG3 H 1.690 0.014 2 96 18 18 ARG HD2 H 3.008 0.006 2 97 18 18 ARG HD3 H 3.165 0.007 2 98 19 19 ALA H H 8.189 0.002 1 99 19 19 ALA HA H 4.177 0.005 1 100 19 19 ALA HB H 1.507 0.008 1 101 20 20 GLN H H 8.184 0.024 1 102 20 20 GLN HA H 3.942 0.007 1 103 20 20 GLN HB2 H 2.064 0.004 2 104 20 20 GLN HB3 H 2.275 0.012 2 105 20 20 GLN HG2 H 2.581 0.003 2 106 20 20 GLN HG3 H 2.581 0.003 2 107 21 21 ASP HA H 4.431 0.008 1 108 21 21 ASP HB2 H 2.776 0.007 2 109 21 21 ASP HB3 H 3.168 0.008 2 110 22 22 PHE H H 8.420 0.000 1 111 22 22 PHE HA H 4.402 0.004 1 112 22 22 PHE HB2 H 3.232 0.023 2 113 22 22 PHE HB3 H 3.321 0.006 2 114 22 22 PHE HD1 H 7.152 0.005 1 115 22 22 PHE HD2 H 7.152 0.005 1 116 22 22 PHE HE1 H 7.222 0.011 1 117 22 22 PHE HE2 H 7.222 0.011 1 118 23 23 VAL H H 8.394 0.002 1 119 23 23 VAL HA H 3.489 0.003 1 120 23 23 VAL HB H 2.143 0.003 1 121 23 23 VAL HG1 H 0.933 0.002 2 122 23 23 VAL HG2 H 1.124 0.038 2 123 24 24 GLN H H 8.157 0.012 1 124 24 24 GLN HA H 3.893 0.007 1 125 24 24 GLN HB2 H 2.088 0.008 2 126 24 24 GLN HB3 H 2.268 0.011 2 127 24 24 GLN HG2 H 2.497 0.004 2 128 24 24 GLN HG3 H 2.497 0.004 2 129 24 24 GLN HE22 H 7.194 0.000 1 130 25 25 TRP H H 8.091 0.071 1 131 25 25 TRP HA H 4.133 0.003 1 132 25 25 TRP HB2 H 3.225 0.004 2 133 25 25 TRP HB3 H 3.554 0.004 2 134 25 25 TRP HE3 H 7.294 0.010 1 135 25 25 TRP HZ3 H 7.021 0.063 1 136 25 25 TRP HH2 H 6.943 0.006 1 137 26 26 LEU H H 8.562 0.002 1 138 26 26 LEU HA H 3.460 0.008 1 139 26 26 LEU HB2 H 1.402 0.007 2 140 26 26 LEU HB3 H 1.621 0.003 2 141 26 26 LEU HG H 1.437 0.045 1 142 26 26 LEU HD1 H 0.678 0.023 2 143 26 26 LEU HD2 H 0.730 0.008 2 144 27 27 MET H H 8.453 0.003 1 145 27 27 MET HA H 4.034 0.004 1 146 27 27 MET HB2 H 1.945 0.014 2 147 27 27 MET HB3 H 2.051 0.005 2 148 27 27 MET HG2 H 2.471 0.002 2 149 27 27 MET HG3 H 2.655 0.003 2 150 28 28 ASN H H 7.718 0.002 1 151 28 28 ASN HA H 4.535 0.004 1 152 28 28 ASN HB2 H 2.647 0.003 2 153 28 28 ASN HB3 H 2.647 0.003 2 154 29 29 THR H H 7.920 0.000 1 155 29 29 THR HA H 4.032 0.011 1 156 29 29 THR HB H 3.636 0.002 1 157 29 29 THR HG2 H 0.648 0.002 1 stop_ save_ save_assigned_chem_shift_list_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H TOCSY' '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 'GGL, 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 1 101 1 GGL HA H 4.369 0.006 1 2 101 1 GGL HB2 H 1.845 0.003 1 3 101 1 GGL HB3 H 2.121 0.007 1 4 101 1 GGL HG H 2.293 0.006 1 stop_ save_ save_assigned_chem_shift_list_1_3 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H TOCSY' '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 'GGL, 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 1 102 1 GGL HA H 4.393 0.004 1 2 102 1 GGL HB2 H 1.856 0.008 1 3 102 1 GGL HB3 H 2.130 0.000 1 4 102 1 GGL HG H 2.222 0.003 1 stop_ save_ save_assigned_chem_shift_list_1_4 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H TOCSY' '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 PLM _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 1 103 1 PLM H13 H 1.305 0.004 1 2 103 1 PLM H14 H 1.245 0.020 1 3 103 1 PLM H15 H 1.169 0.012 1 4 103 1 PLM H16 H 0.753 0.005 1 5 103 1 PLM H2 H 2.162 0.008 1 6 103 1 PLM H3 H 1.497 0.008 1 7 103 1 PLM H4 H 1.207 0.005 1 stop_ save_