data_5246 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Chiral Mutagenesis of Insulin's Hidden Receptor-Binding Surface: Structure of an Allo-isoleucine A2 Analogue ; _BMRB_accession_number 5246 _BMRB_flat_file_name bmr5246.str _Entry_type original _Submission_date 2001-12-27 _Accession_date 2001-12-27 _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 Xu Bin . . 2 Hua Qing-xin . . 3 Nakagawa Satoe H. . 4 Jia Wenhua . . 5 Chu Ying-Chi . . 6 Katsoyannis Panayotis G. . 7 Weiss Michael A. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 4 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 475 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2008-07-17 update BMRB 'Updating non-standard residue' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Chiral Mutagenesis of Insulin's Hidden Receptor-binding Surface: Structure of an Allo-isoleucine(A2) Analogue ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code 21856752 _PubMed_ID 11866509 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Xu Bin . . 2 Hua Qing-xin . . 3 Nakagawa Satoe H. . 4 Jia Wenhua . . 5 Chu Ying-Chi . . 6 Katsoyannis Panayotis G. . 7 Weiss Michael A. . stop_ _Journal_abbreviation 'J. Mol. Biol.' _Journal_volume 316 _Journal_issue 3 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 435 _Page_last 441 _Year 2002 _Details . loop_ _Keyword 'protein folding' insulin 'insulin analogues' 'insulin receptor' 'insulin chain combination' stop_ save_ ################################## # Molecular system description # ################################## save_system_HI _Saveframe_category molecular_system _Mol_system_name 'Human insulin mutant' _Abbreviation_common HI _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'allo-IleA2-DKP-insulin, chain A' $HI_A 'allo-IleA2-DKP-insulin, chain B' $HI_B stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state dimer _System_paramagnetic no _System_thiol_state 'all disulfide bound' loop_ _Biological_function hormone 'glucose metabolism' 'disease mutation' diabetes stop_ _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_HI_A _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common 'human insulin' _Name_variant 'Ile-A2-allo-Ile, His-B10-Asp, Pro-B28-Lys, Lys-B29-Pro' _Abbreviation_common HI _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 21 _Mol_residue_sequence ; GXVEQCCTSICSLYQLENYC N ; loop_ _Residue_seq_code _Residue_label 1 GLY 2 IIL 3 VAL 4 GLU 5 GLN 6 CYS 7 CYS 8 THR 9 SER 10 ILE 11 CYS 12 SER 13 LEU 14 TYR 15 GLN 16 LEU 17 GLU 18 ASN 19 TYR 20 CYS 21 ASN stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2015-01-28 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 15450 B-chain 100.00 30 100.00 100.00 8.07e-13 BMRB 15454 B_chain 100.00 30 100.00 100.00 8.07e-13 BMRB 15455 B_chain 100.00 30 100.00 100.00 8.07e-13 BMRB 16608 Proinsulin 100.00 86 100.00 100.00 1.28e-12 BMRB 17108 "Human Insulin" 100.00 30 100.00 100.00 8.07e-13 BMRB 1760 "insulin B chain" 100.00 30 100.00 100.00 8.07e-13 BMRB 1762 "insulin B chain" 100.00 30 100.00 100.00 8.07e-13 PDB 1K3M "Nmr Structure Of Human Insulin Mutant Ile-A2-Ala, His-B10- Asp, Pro-B28-Lys, Lys-B29-Pro, 15 Structures" 100.00 30 100.00 100.00 8.07e-13 PDB 1KMF "Nmr Structure Of Human Insulin Mutant Ile-A2-Allo-Ile, His- B10-Asp, Pro-B28-Lys, Lys-B29-Pro, 15 Structures" 100.00 30 100.00 100.00 8.07e-13 PDB 1LKQ "Nmr Structure Of Human Insulin Mutant Ile-A2-Gly, Val-A3- Gly, His-B10-Asp, Pro-B28-Lys, Lys-B29-Pro, 20 Structures" 100.00 30 100.00 100.00 8.07e-13 PDB 1VKT "Human Insulin Two Disulfide Model, Nmr, 10 Structures" 100.00 30 100.00 100.00 8.07e-13 PDB 2JMN "Nmr Structure Of Human Insulin Mutant His-B10-Asp, Pro-B28- Lys, Lys-B29-Pro, 20 Structures" 100.00 30 100.00 100.00 8.07e-13 PDB 2JUM Thra3-Dkp-Insulin 100.00 30 100.00 100.00 8.07e-13 PDB 2JUU "Allo-Thra3 Dkp-Insulin" 100.00 30 100.00 100.00 8.07e-13 PDB 2JUV Abaa3-Dkp-Insulin 100.00 30 100.00 100.00 8.07e-13 PDB 2KQP "Nmr Structure Of Proinsulin" 100.00 86 100.00 100.00 1.28e-12 PDB 2L1Z "Nmr Structure Of Human Insulin Mutant Gly-B20-D-Ala, Gly-B23-D-Ala Pro-B28-Lys, Lys-B29-Pro, 20 Structures" 100.00 30 100.00 100.00 8.07e-13 PDB 4IUZ "High Resolution Crystal Structure Of Racemic Ester Insulin" 100.00 30 100.00 100.00 8.07e-13 stop_ save_ save_HI_B _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common 'human insulin' _Name_variant 'Ile-A2-allo-Ile, His-B10-Asp, Pro-B28-Lys, Lys-B29-Pro' _Abbreviation_common HI _Molecular_mass . _Mol_thiol_state 'all disulfide bound' _Details . _Residue_count 30 _Mol_residue_sequence ; FVNQHLCGSDLVEALYLVCG ERGFFYTKPT ; loop_ _Residue_seq_code _Residue_label 1 PHE 2 VAL 3 ASN 4 GLN 5 HIS 6 LEU 7 CYS 8 GLY 9 SER 10 ASP 11 LEU 12 VAL 13 GLU 14 ALA 15 LEU 16 TYR 17 LEU 18 VAL 19 CYS 20 GLY 21 GLU 22 ARG 23 GLY 24 PHE 25 PHE 26 TYR 27 THR 28 LYS 29 PRO 30 THR stop_ _Sequence_homology_query_date 2008-03-24 _Sequence_homology_query_revised_last_date 2008-01-16 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 1760 'insulin B chain' 100.00 30 100 100 10e-11 BMRB 1762 'insulin B chain' 100.00 30 100 100 10e-11 PDB 1SJT 'B Chain B, Mini-Proinsulin, Two ChainInsulin Analog Mutant: Des B30, His(B 10)asp, Pro(B28)asp, Nmr, 20 Structures' 103.45 29 100 100 10e-09 PDB 1K3M 'B Chain B, Nmr Structure Of Human InsulinMutant Ile-A2-Ala, His-B10- Asp, Pro-B28-Lys,Lys-B29-Pro, 15 Structures' 100.00 30 100 100 10e-11 PDB 1KMF 'B Chain B, Nmr Structure Of Human InsulinMutant Ile-A2-Allo-Ile, His- B10-Asp, Pro-B28-Lys,Lys-B29-Pro, 15 Structures' 100.00 30 100 100 10e-11 PDB 1LKQ 'B Chain B, Nmr Structure Of Human InsulinMutant Ile-A2-Gly, Val-A3- Gly, His-B10-Asp,Pro-B28-Lys, Lys-B29-Pro, 20 Struct' 100.00 30 100 100 10e-11 PDB 1VKT 'B Chain B, Human Insulin Two DisulfideModel, Nmr, 10 Structures' 100.00 30 100 100 10e-11 PDB 2JMN 'B Chain B, Nmr Structure Of Human InsulinMutant His-B10-Asp, Pro-B28- Lys, Lys-B29-Pro, 20Structures' 100.00 30 100 100 10e-11 PDB 2JUM 'B Chain B, Thra3-Dkp-Insulin' 100.00 30 100 100 10e-11 PDB 2JUU 'B Chain B, Allo-Thra3 Dkp-Insulin' 100.00 30 100 100 10e-11 PDB 2JUV 'B Chain B, Abaa3-Dkp-Insulin' 100.00 30 100 100 10e-11 PDB 1SJU 'A Chain A, Mini-Proinsulin, Single ChainInsulin Analog Mutant: Des B30, His(B 10)asp, Pro(B28)asp And Peptide Bond Betwe' 60.00 50 100 100 10e-09 stop_ save_ ###################### # Polymer residues # ###################### save_chem_comp_IIL _Saveframe_category polymer_residue _Mol_type 'L-peptide linking' _Name_common ISO-ISOLEUCINE _BMRB_code . _PDB_code IIL _Standard_residue_derivative . _Molecular_mass 131.173 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Fri Jul 22 11:13:42 2011 ; 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 . ? CG2 CG2 C . 0 . ? CG1 CG1 C . 0 . ? CD1 CD1 C . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB HB H . 0 . ? HG21 HG21 H . 0 . ? HG22 HG22 H . 0 . ? HG23 HG23 H . 0 . ? HG12 HG12 H . 0 . ? HG13 HG13 H . 0 . ? HD11 HD11 H . 0 . ? HD12 HD12 H . 0 . ? HD13 HD13 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 CG2 ? ? SING CB CG1 ? ? SING CB HB ? ? SING CG2 HG21 ? ? SING CG2 HG22 ? ? SING CG2 HG23 ? ? SING CG1 CD1 ? ? SING CG1 HG12 ? ? SING CG1 HG13 ? ? SING CD1 HD11 ? ? SING CD1 HD12 ? ? SING CD1 HD13 ? ? SING OXT HXT ? ? stop_ save_ ######################################## # Molecular bond linkage definitions # ######################################## save_crosslink_bonds _Saveframe_category crosslink_bonds loop_ _Bond_order _Bond_type _Atom_one_mol_system_component_name _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_atom_name _Atom_two_mol_system_component_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_atom_name single disulfide 'allo-IleA2-DKP-insulin, chain A' 20 CYS SG 'allo-IleA2-DKP-insulin, chain B' 19 CYS SG single disulfide 'allo-IleA2-DKP-insulin, chain A' 7 CYS SG 'allo-IleA2-DKP-insulin, chain B' 7 CYS SG single disulfide 'allo-IleA2-DKP-insulin, chain A' 6 CYS SG 'allo-IleA2-DKP-insulin, chain A' 11 CYS SG stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $HI_A Human 9606 Eukaryota Metazoa Homo sapiens $HI_B Human 9606 Eukaryota Metazoa Homo sapiens stop_ save_ ######################### # Experimental source # ######################### save_experimental_source _Saveframe_category experimental_source loop_ _Mol_label _Production_method _Host_organism_name_common _Genus _Species _Strain _Vector_name $HI_A 'chemical synthesis' . . . . . $HI_B '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 _Concentration_min_value _Concentration_max_value _Isotopic_labeling $HI_A 1.2 mM 1.0 3.0 . $HI_B 1.2 mM 1.0 3.0 . stop_ save_ ############################ # Computer software used # ############################ save_VNMR _Saveframe_category software _Name VNMR _Version 6.1B loop_ _Task 'NMR data processing' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_1H-1H_DQF-COSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H DQF-COSY' _Sample_label $sample_1 save_ save_NMR_applied_experiment _Saveframe_category NMR_applied_experiment _Experiment_name . _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H DQF-COSY' _BMRB_pulse_sequence_accession_number . _Details . save_ ####################### # Sample conditions # ####################### save_cond_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 7.0 0.1 n/a temperature 298 1 K stop_ save_ save_cond_2 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pD 7.6 0.1 n/a temperature 305 1 K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference _Saveframe_category chemical_shift_reference _Details . loop_ _Mol_common_name _Atom_type _Atom_isotope_number _Atom_group _Chem_shift_units _Chem_shift_value _Reference_method _Reference_type _External_reference_sample_geometry _External_reference_location _External_reference_axis _Indirect_shift_ratio DSS H 1 'methyl protons' ppm 0.0 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_shift_set_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $cond_1 _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name 'allo-IleA2-DKP-insulin, chain A' _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 . 2 IIL H H 8.39 0.02 1 2 . 2 IIL HA H 3.83 0.02 1 3 . 2 IIL HB H 1.98 0.02 1 4 . 2 IIL HG12 H 1.02 0.02 1 5 . 2 IIL HG13 H 1.02 0.02 1 6 . 2 IIL HG2 H 0.64 0.02 1 7 . 2 IIL HD1 H 0.51 0.02 1 8 . 3 VAL H H 8.33 0.02 1 9 . 3 VAL HA H 3.54 0.02 1 10 . 3 VAL HB H 1.98 0.02 1 11 . 3 VAL HG1 H 1.02 0.02 2 12 . 3 VAL HG2 H 0.91 0.02 2 13 . 4 GLU H H 8.40 0.02 1 14 . 4 GLU HA H 4.11 0.02 1 15 . 4 GLU HB2 H 2.19 0.02 2 16 . 4 GLU HB3 H 2.02 0.02 2 17 . 4 GLU HG2 H 2.52 0.02 2 18 . 4 GLU HG3 H 2.31 0.02 2 19 . 5 GLN H H 8.40 0.02 1 20 . 5 GLN HA H 4.11 0.02 1 21 . 5 GLN HB2 H 2.19 0.02 2 22 . 5 GLN HB3 H 2.02 0.02 2 23 . 5 GLN HG2 H 2.52 0.02 2 24 . 5 GLN HG3 H 2.29 0.02 2 25 . 6 CYS H H 8.32 0.02 1 26 . 6 CYS HA H 4.98 0.02 1 27 . 6 CYS HB2 H 3.19 0.02 2 28 . 6 CYS HB3 H 2.90 0.02 2 29 . 7 CYS H H 8.37 0.02 1 30 . 7 CYS HA H 4.90 0.02 1 31 . 7 CYS HB2 H 3.88 0.02 2 32 . 7 CYS HB3 H 3.46 0.02 2 33 . 8 THR H H 8.28 0.02 1 34 . 8 THR HA H 4.00 0.02 1 35 . 8 THR HB H 4.49 0.02 1 36 . 8 THR HG2 H 1.28 0.02 1 37 . 9 SER HA H 4.76 0.02 1 38 . 9 SER HB2 H 4.07 0.02 2 39 . 9 SER HB3 H 3.86 0.02 2 40 . 10 ILE H H 7.77 0.02 1 41 . 10 ILE HA H 4.38 0.02 1 42 . 10 ILE HB H 1.50 0.02 1 43 . 10 ILE HG12 H 1.23 0.02 2 44 . 10 ILE HG13 H 0.32 0.02 2 45 . 10 ILE HG2 H 0.63 0.02 1 46 . 10 ILE HD1 H 0.50 0.02 1 47 . 11 CYS H H 9.92 0.02 1 48 . 11 CYS HA H 5.13 0.02 1 49 . 11 CYS HB2 H 3.10 0.02 2 50 . 11 CYS HB3 H 2.90 0.02 2 51 . 12 SER H H 8.55 0.02 1 52 . 12 SER HA H 4.63 0.02 1 53 . 12 SER HB2 H 4.15 0.02 2 54 . 12 SER HB3 H 3.97 0.02 2 55 . 13 LEU H H 8.75 0.02 1 56 . 13 LEU HA H 3.90 0.02 1 57 . 13 LEU HB2 H 1.56 0.02 2 58 . 13 LEU HB3 H 1.44 0.02 2 59 . 13 LEU HG H 1.39 0.02 1 60 . 13 LEU HD1 H 0.82 0.02 1 61 . 13 LEU HD2 H 0.71 0.02 1 62 . 14 TYR H H 7.63 0.02 1 63 . 14 TYR HA H 4.31 0.02 1 64 . 14 TYR HB2 H 3.00 0.02 1 65 . 14 TYR HB3 H 3.00 0.02 1 66 . 14 TYR HD1 H 7.11 0.02 1 67 . 14 TYR HE1 H 6.85 0.02 1 68 . 15 GLN H H 7.54 0.02 1 69 . 15 GLN HA H 3.99 0.02 1 70 . 15 GLN HB2 H 2.05 0.02 2 71 . 15 GLN HB3 H 1.95 0.02 2 72 . 15 GLN HG2 H 2.41 0.02 2 73 . 15 GLN HG3 H 2.24 0.02 2 74 . 16 LEU H H 7.89 0.02 1 75 . 16 LEU HA H 4.11 0.02 1 76 . 16 LEU HB2 H 1.95 0.02 2 77 . 16 LEU HB3 H 1.51 0.02 2 78 . 16 LEU HG H 1.71 0.02 1 79 . 16 LEU HD1 H 0.78 0.02 1 80 . 16 LEU HD2 H 0.71 0.02 1 81 . 17 GLU H H 7.90 0.02 1 82 . 17 GLU HA H 4.20 0.02 1 83 . 17 GLU HB2 H 2.02 0.02 2 84 . 17 GLU HB3 H 1.95 0.02 2 85 . 17 GLU HG2 H 2.36 0.02 2 86 . 17 GLU HG3 H 2.28 0.02 2 87 . 18 ASN H H 7.32 0.02 1 88 . 18 ASN HA H 4.44 0.02 1 89 . 18 ASN HB2 H 2.60 0.02 2 90 . 18 ASN HB3 H 2.47 0.02 2 91 . 19 TYR H H 7.90 0.02 1 92 . 19 TYR HA H 4.19 0.02 1 93 . 19 TYR HB2 H 3.52 0.02 2 94 . 19 TYR HB3 H 2.65 0.02 2 95 . 19 TYR HD1 H 7.25 0.02 1 96 . 19 TYR HE1 H 6.74 0.02 1 97 . 20 CYS H H 7.22 0.02 1 98 . 20 CYS HA H 5.13 0.02 1 99 . 20 CYS HB2 H 3.33 0.02 2 100 . 20 CYS HB3 H 2.82 0.02 2 101 . 21 ASN H H 8.06 0.02 1 102 . 21 ASN HA H 4.52 0.02 1 103 . 21 ASN HB2 H 2.79 0.02 2 104 . 21 ASN HB3 H 2.61 0.02 2 105 . 21 ASN HD21 H 7.54 0.02 1 stop_ save_ save_shift_set_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $cond_1 _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name 'allo-IleA2-DKP-insulin, chain B' _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 PHE HA H 4.15 0.02 1 2 . 1 PHE HB2 H 3.75 0.02 2 3 . 1 PHE HB3 H 3.15 0.02 2 4 . 1 PHE HD1 H 7.23 0.02 1 5 . 1 PHE HE1 H 7.32 0.02 1 6 . 2 VAL H H 8.24 0.02 1 7 . 2 VAL HA H 4.07 0.02 1 8 . 2 VAL HB H 2.06 0.02 1 9 . 2 VAL HG1 H 0.86 0.02 1 10 . 3 ASN H H 8.55 0.02 1 11 . 3 ASN HA H 4.63 0.02 1 12 . 3 ASN HB2 H 2.82 0.02 2 13 . 3 ASN HB3 H 2.71 0.02 2 14 . 4 GLN H H 8.23 0.02 1 15 . 4 GLN HA H 4.49 0.02 1 16 . 4 GLN HB2 H 2.10 0.02 2 17 . 4 GLN HB3 H 1.93 0.02 2 18 . 4 GLN HG2 H 2.18 0.02 2 19 . 4 GLN HG3 H 2.08 0.02 2 20 . 5 HIS H H 8.55 0.02 1 21 . 5 HIS HA H 4.38 0.02 1 22 . 5 HIS HB2 H 3.52 0.02 2 23 . 5 HIS HB3 H 3.18 0.02 2 24 . 6 LEU H H 9.07 0.02 1 25 . 6 LEU HA H 4.59 0.02 1 26 . 6 LEU HB2 H 1.71 0.02 2 27 . 6 LEU HB3 H 0.72 0.02 2 28 . 6 LEU HG H 1.59 0.02 1 29 . 6 LEU HD1 H 0.80 0.02 2 30 . 6 LEU HD2 H 0.72 0.02 2 31 . 7 CYS H H 8.71 0.02 1 32 . 7 CYS HA H 5.00 0.02 1 33 . 7 CYS HB2 H 3.22 0.02 2 34 . 7 CYS HB3 H 2.92 0.02 2 35 . 8 GLY H H 9.44 0.02 1 36 . 8 GLY HA2 H 3.99 0.02 2 37 . 8 GLY HA3 H 3.89 0.02 2 38 . 9 SER H H 9.10 0.02 1 39 . 9 SER HA H 4.20 0.02 1 40 . 9 SER HB2 H 3.83 0.02 1 41 . 9 SER HB3 H 3.83 0.02 1 42 . 10 ASP H H 7.97 0.02 1 43 . 10 ASP HA H 4.41 0.02 1 44 . 10 ASP HB2 H 3.06 0.02 2 45 . 10 ASP HB3 H 2.65 0.02 2 46 . 11 LEU H H 6.84 0.02 1 47 . 11 LEU HA H 3.89 0.02 1 48 . 11 LEU HB2 H 1.88 0.02 2 49 . 11 LEU HB3 H 1.17 0.02 2 50 . 11 LEU HG H 1.24 0.02 1 51 . 11 LEU HD1 H 0.79 0.02 2 52 . 11 LEU HD2 H 0.73 0.02 2 53 . 12 VAL H H 6.82 0.02 1 54 . 12 VAL HA H 3.32 0.02 1 55 . 12 VAL HB H 2.09 0.02 1 56 . 12 VAL HG1 H 0.99 0.02 1 57 . 13 GLU H H 8.06 0.02 1 58 . 13 GLU HA H 4.05 0.02 1 59 . 13 GLU HB2 H 2.13 0.02 2 60 . 13 GLU HB3 H 2.09 0.02 2 61 . 13 GLU HG2 H 2.60 0.02 2 62 . 13 GLU HG3 H 2.43 0.02 2 63 . 14 ALA H H 7.67 0.02 1 64 . 14 ALA HA H 4.05 0.02 1 65 . 14 ALA HB H 1.37 0.02 1 66 . 15 LEU H H 8.07 0.02 1 67 . 15 LEU HA H 3.71 0.02 1 68 . 15 LEU HB2 H 1.06 0.02 2 69 . 15 LEU HB3 H 0.27 0.02 2 70 . 15 LEU HG H 1.23 0.02 1 71 . 15 LEU HD1 H 0.52 0.02 2 72 . 15 LEU HD2 H -0.02 0.02 2 73 . 16 TYR H H 8.29 0.02 1 74 . 16 TYR HA H 4.38 0.02 1 75 . 16 TYR HB2 H 3.17 0.02 2 76 . 16 TYR HB3 H 3.13 0.02 2 77 . 16 TYR HD1 H 7.21 0.02 1 78 . 16 TYR HE1 H 6.80 0.02 1 79 . 17 LEU H H 7.72 0.02 1 80 . 17 LEU HA H 4.07 0.02 1 81 . 17 LEU HB2 H 1.90 0.02 2 82 . 17 LEU HB3 H 1.76 0.02 2 83 . 17 LEU HG H 1.78 0.02 1 84 . 17 LEU HD1 H 0.93 0.02 2 85 . 17 LEU HD2 H 0.90 0.02 2 86 . 18 VAL H H 8.34 0.02 1 87 . 18 VAL HA H 3.77 0.02 1 88 . 18 VAL HB H 1.98 0.02 1 89 . 18 VAL HG1 H 1.01 0.02 2 90 . 18 VAL HG2 H 0.89 0.02 2 91 . 19 CYS H H 8.84 0.02 1 92 . 19 CYS HA H 4.84 0.02 1 93 . 19 CYS HB2 H 3.32 0.02 2 94 . 19 CYS HB3 H 2.88 0.02 2 95 . 20 GLY H H 7.79 0.02 1 96 . 20 GLY HA2 H 3.99 0.02 2 97 . 20 GLY HA3 H 3.83 0.02 2 98 . 21 GLU H H 9.11 0.02 1 99 . 21 GLU HA H 4.20 0.02 1 100 . 21 GLU HB2 H 2.21 0.02 2 101 . 21 GLU HB3 H 2.06 0.02 2 102 . 21 GLU HG2 H 2.38 0.02 1 103 . 22 ARG H H 8.12 0.02 1 104 . 22 ARG HA H 4.19 0.02 1 105 . 22 ARG HB2 H 2.16 0.02 2 106 . 22 ARG HB3 H 2.06 0.02 2 107 . 22 ARG HG2 H 1.90 0.02 2 108 . 22 ARG HG3 H 1.85 0.02 2 109 . 22 ARG HD2 H 3.39 0.02 2 110 . 22 ARG HD3 H 3.32 0.02 2 111 . 23 GLY H H 7.37 0.02 1 112 . 23 GLY HA2 H 4.13 0.02 2 113 . 23 GLY HA3 H 3.80 0.02 2 114 . 24 PHE H H 7.55 0.02 1 115 . 24 PHE HA H 5.31 0.02 1 116 . 24 PHE HB2 H 3.07 0.02 2 117 . 24 PHE HB3 H 2.87 0.02 2 118 . 24 PHE HD1 H 6.66 0.02 1 119 . 24 PHE HE1 H 6.82 0.02 1 120 . 25 PHE H H 8.56 0.02 1 121 . 25 PHE HA H 4.94 0.02 1 122 . 25 PHE HB2 H 3.19 0.02 2 123 . 25 PHE HB3 H 3.04 0.02 2 124 . 25 PHE HD1 H 7.19 0.02 1 125 . 25 PHE HE1 H 7.26 0.02 1 126 . 26 TYR H H 8.31 0.02 1 127 . 26 TYR HA H 4.57 0.02 1 128 . 26 TYR HB2 H 2.89 0.02 1 129 . 26 TYR HD1 H 7.10 0.02 1 130 . 26 TYR HE1 H 6.76 0.02 1 131 . 27 THR H H 7.80 0.02 1 132 . 27 THR HA H 4.59 0.02 1 133 . 27 THR HB H 4.13 0.02 1 134 . 27 THR HG2 H 1.20 0.02 1 135 . 28 LYS H H 8.54 0.02 1 136 . 28 LYS HA H 4.38 0.02 1 137 . 28 LYS HB2 H 1.80 0.02 2 138 . 28 LYS HB3 H 1.70 0.02 2 139 . 28 LYS HG2 H 1.42 0.02 1 140 . 28 LYS HD2 H 1.62 0.02 1 141 . 28 LYS HE2 H 2.89 0.02 1 142 . 29 PRO HA H 4.47 0.02 1 143 . 29 PRO HB2 H 2.29 0.02 2 144 . 29 PRO HB3 H 1.97 0.02 2 145 . 29 PRO HG2 H 1.97 0.02 1 146 . 29 PRO HD2 H 3.63 0.02 2 147 . 29 PRO HD3 H 3.53 0.02 2 148 . 30 THR H H 7.80 0.02 1 149 . 30 THR HA H 4.13 0.02 1 150 . 30 THR HB H 4.23 0.02 1 151 . 30 THR HG2 H 1.20 0.02 1 stop_ save_ save_shift_set_3 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $cond_2 _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name 'allo-IleA2-DKP-insulin, chain A' _Text_data_format . _Text_data . loop_ _Atom_shift_assign_ID _Residue_author_seq_code _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 . 2 IIL HA H 3.90 0.02 1 2 . 2 IIL HB H 1.47 0.02 1 3 . 2 IIL HG12 H 1.50 0.02 2 4 . 2 IIL HG13 H 1.03 0.02 2 5 . 2 IIL HG2 H 0.68 0.02 1 6 . 2 IIL HD1 H 0.50 0.02 1 7 . 3 VAL HA H 3.57 0.02 1 8 . 3 VAL HB H 1.96 0.02 1 9 . 3 VAL HG1 H 1.02 0.02 2 10 . 3 VAL HG2 H 0.89 0.02 2 11 . 5 GLN HA H 4.10 0.02 1 12 . 5 GLN HB2 H 2.14 0.02 2 13 . 5 GLN HB3 H 2.00 0.02 2 14 . 5 GLN HG2 H 2.23 0.02 1 15 . 6 CYS H H 8.26 0.02 1 16 . 6 CYS HA H 4.95 0.02 1 17 . 6 CYS HB2 H 3.20 0.02 2 18 . 6 CYS HB3 H 2.86 0.02 2 19 . 7 CYS HA H 4.88 0.02 1 20 . 7 CYS HB2 H 3.83 0.02 2 21 . 7 CYS HB3 H 3.40 0.02 2 22 . 8 THR HA H 4.07 0.02 1 23 . 8 THR HB H 4.66 0.02 1 24 . 8 THR HG2 H 1.25 0.02 1 25 . 9 SER HA H 4.70 0.02 1 26 . 9 SER HB2 H 3.95 0.02 2 27 . 9 SER HB3 H 3.80 0.02 2 28 . 10 ILE HA H 4.33 0.02 1 29 . 10 ILE HB H 1.51 0.02 1 30 . 10 ILE HG12 H 1.12 0.02 1 31 . 10 ILE HG13 H 1.12 0.02 1 32 . 10 ILE HG2 H 0.62 0.02 1 33 . 10 ILE HD1 H 0.50 0.02 1 34 . 12 SER HA H 4.62 0.02 1 35 . 12 SER HB2 H 4.07 0.02 2 36 . 12 SER HB3 H 3.94 0.02 2 37 . 13 LEU H H 8.73 0.02 1 38 . 13 LEU HA H 3.97 0.02 1 39 . 13 LEU HB2 H 1.53 0.02 2 40 . 13 LEU HB3 H 1.48 0.02 2 41 . 13 LEU HG H 1.53 0.02 1 42 . 13 LEU HD1 H 0.90 0.02 1 43 . 13 LEU HD2 H 0.82 0.02 1 44 . 14 TYR H H 7.57 0.02 1 45 . 14 TYR HA H 4.36 0.02 1 46 . 14 TYR HB2 H 3.01 0.02 1 47 . 14 TYR HB3 H 3.01 0.02 1 48 . 14 TYR HD1 H 7.12 0.02 1 49 . 14 TYR HE1 H 6.85 0.02 1 50 . 15 GLN H H 7.53 0.02 1 51 . 15 GLN HA H 4.00 0.02 1 52 . 15 GLN HG2 H 2.37 0.02 2 53 . 15 GLN HG3 H 2.19 0.02 2 54 . 16 LEU H H 7.85 0.02 1 55 . 16 LEU HA H 4.10 0.02 1 56 . 16 LEU HB2 H 1.96 0.02 2 57 . 16 LEU HB3 H 1.48 0.02 2 58 . 16 LEU HG H 1.71 0.02 1 59 . 16 LEU HD1 H 0.74 0.02 1 60 . 16 LEU HD2 H 0.68 0.02 1 61 . 17 GLU H H 7.87 0.02 1 62 . 17 GLU HA H 4.18 0.02 1 63 . 17 GLU HB2 H 1.99 0.02 1 64 . 17 GLU HB3 H 1.99 0.02 1 65 . 17 GLU HG2 H 2.36 0.02 2 66 . 17 GLU HG3 H 2.20 0.02 2 67 . 18 ASN H H 7.32 0.02 1 68 . 18 ASN HA H 4.43 0.02 1 69 . 18 ASN HB2 H 2.57 0.02 2 70 . 18 ASN HB3 H 2.47 0.02 2 71 . 19 TYR H H 7.87 0.02 1 72 . 19 TYR HA H 4.20 0.02 1 73 . 19 TYR HB2 H 3.52 0.02 2 74 . 19 TYR HB3 H 2.63 0.02 2 75 . 19 TYR HD1 H 7.23 0.02 1 76 . 19 TYR HE1 H 6.74 0.02 1 77 . 20 CYS H H 7.17 0.02 1 78 . 20 CYS HA H 5.12 0.02 1 79 . 20 CYS HB2 H 3.30 0.02 2 80 . 20 CYS HB3 H 2.78 0.02 2 81 . 21 ASN H H 8.02 0.02 1 82 . 21 ASN HA H 4.50 0.02 1 83 . 21 ASN HB2 H 2.77 0.02 2 84 . 21 ASN HB3 H 2.58 0.02 2 85 . 21 ASN HD21 H 7.47 0.02 2 86 . 21 ASN HD22 H 6.38 0.02 2 stop_ save_ save_shift_set_4 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $cond_2 _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name 'allo-IleA2-DKP-insulin, chain B' _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 PHE HA H 3.94 0.02 1 2 . 1 PHE HB2 H 3.20 0.02 2 3 . 1 PHE HB3 H 3.03 0.02 2 4 . 3 ASN HA H 4.57 0.02 1 5 . 3 ASN HB2 H 2.83 0.02 2 6 . 3 ASN HB3 H 2.73 0.02 2 7 . 4 GLN HA H 4.47 0.02 1 8 . 4 GLN HB2 H 1.92 0.02 1 9 . 4 GLN HG2 H 2.10 0.02 1 10 . 5 HIS HA H 4.34 0.02 1 11 . 5 HIS HB2 H 3.44 0.02 2 12 . 5 HIS HB3 H 3.08 0.02 2 13 . 6 LEU H H 8.92 0.02 1 14 . 6 LEU HA H 4.57 0.02 1 15 . 6 LEU HB2 H 1.70 0.02 2 16 . 6 LEU HB3 H 0.80 0.02 2 17 . 6 LEU HG H 1.54 0.02 1 18 . 6 LEU HD1 H 0.90 0.02 2 19 . 6 LEU HD2 H 0.80 0.02 2 20 . 7 CYS H H 8.63 0.02 1 21 . 7 CYS HA H 4.98 0.02 1 22 . 7 CYS HB2 H 3.22 0.02 2 23 . 7 CYS HB3 H 2.93 0.02 2 24 . 8 GLY HA2 H 4.00 0.02 2 25 . 8 GLY HA3 H 3.86 0.02 2 26 . 9 SER HA H 4.15 0.02 1 27 . 9 SER HB2 H 4.02 0.02 2 28 . 9 SER HB3 H 3.92 0.02 2 29 . 10 ASP H H 7.98 0.02 1 30 . 10 ASP HA H 4.38 0.02 1 31 . 10 ASP HB2 H 3.00 0.02 2 32 . 10 ASP HB3 H 2.65 0.02 2 33 . 11 LEU H H 6.93 0.02 1 34 . 11 LEU HA H 3.88 0.02 1 35 . 11 LEU HB2 H 1.85 0.02 2 36 . 11 LEU HB3 H 1.16 0.02 2 37 . 11 LEU HG H 1.23 0.02 1 38 . 11 LEU HD1 H 0.75 0.02 2 39 . 11 LEU HD2 H 0.63 0.02 2 40 . 12 VAL H H 7.13 0.02 1 41 . 12 VAL HA H 3.20 0.02 1 42 . 12 VAL HB H 2.09 0.02 1 43 . 12 VAL HG1 H 1.06 0.02 2 44 . 12 VAL HG2 H 0.98 0.02 2 45 . 13 GLU HA H 4.06 0.02 1 46 . 13 GLU HB2 H 2.13 0.02 2 47 . 13 GLU HB3 H 2.07 0.02 2 48 . 13 GLU HG2 H 2.54 0.02 1 49 . 14 ALA H H 7.56 0.02 1 50 . 14 ALA HA H 4.13 0.02 1 51 . 14 ALA HB H 1.40 0.02 1 52 . 15 LEU H H 8.03 0.02 1 53 . 15 LEU HA H 3.72 0.02 1 54 . 15 LEU HB2 H 1.07 0.02 2 55 . 15 LEU HB3 H 0.28 0.02 2 56 . 15 LEU HG H 1.20 0.02 1 57 . 15 LEU HD1 H 0.50 0.02 2 58 . 15 LEU HD2 H -0.02 0.02 2 59 . 16 TYR H H 8.23 0.02 1 60 . 16 TYR HA H 4.38 0.02 1 61 . 16 TYR HB2 H 3.15 0.02 1 62 . 16 TYR HB3 H 3.15 0.02 1 63 . 16 TYR HD1 H 7.23 0.02 1 64 . 16 TYR HE1 H 6.78 0.02 1 65 . 17 LEU H H 7.63 0.02 1 66 . 17 LEU HA H 4.08 0.02 1 67 . 17 LEU HB2 H 1.90 0.02 2 68 . 17 LEU HB3 H 1.77 0.02 2 69 . 17 LEU HG H 1.77 0.02 1 70 . 17 LEU HD1 H 0.94 0.02 1 71 . 17 LEU HD2 H 0.94 0.02 1 72 . 18 VAL H H 8.17 0.02 1 73 . 18 VAL HA H 3.82 0.02 1 74 . 18 VAL HB H 1.97 0.02 1 75 . 18 VAL HG1 H 1.04 0.02 2 76 . 18 VAL HG2 H 0.89 0.02 2 77 . 19 CYS H H 8.82 0.02 1 78 . 19 CYS HA H 4.80 0.02 1 79 . 19 CYS HB2 H 3.30 0.02 2 80 . 19 CYS HB3 H 2.83 0.02 2 81 . 20 GLY H H 7.78 0.02 1 82 . 20 GLY HA2 H 4.03 0.02 2 83 . 20 GLY HA3 H 3.93 0.02 2 84 . 21 GLU HA H 4.10 0.02 1 85 . 21 GLU HB2 H 2.16 0.02 1 86 . 21 GLU HG2 H 2.26 0.02 1 87 . 22 ARG H H 8.07 0.02 1 88 . 22 ARG HA H 4.15 0.02 1 89 . 22 ARG HB2 H 2.13 0.02 2 90 . 22 ARG HB3 H 2.07 0.02 2 91 . 22 ARG HG2 H 1.85 0.02 1 92 . 22 ARG HG3 H 1.85 0.02 1 93 . 22 ARG HD2 H 3.37 0.02 2 94 . 22 ARG HD3 H 3.30 0.02 2 95 . 23 GLY H H 7.34 0.02 1 96 . 23 GLY HA2 H 4.15 0.02 2 97 . 23 GLY HA3 H 3.80 0.02 2 98 . 24 PHE H H 7.53 0.02 1 99 . 24 PHE HA H 5.30 0.02 1 100 . 24 PHE HB2 H 3.08 0.02 2 101 . 24 PHE HB3 H 2.86 0.02 2 102 . 24 PHE HD1 H 6.63 0.02 1 103 . 24 PHE HE1 H 6.79 0.02 1 104 . 25 PHE H H 8.53 0.02 1 105 . 25 PHE HA H 4.80 0.02 1 106 . 25 PHE HB2 H 3.27 0.02 2 107 . 25 PHE HB3 H 3.18 0.02 2 108 . 25 PHE HD1 H 7.19 0.02 1 109 . 25 PHE HE1 H 7.27 0.02 1 110 . 26 TYR H H 8.26 0.02 1 111 . 26 TYR HA H 4.55 0.02 1 112 . 26 TYR HB2 H 3.01 0.02 1 113 . 26 TYR HD1 H 7.13 0.02 1 114 . 26 TYR HE1 H 6.74 0.02 1 115 . 27 THR H H 7.73 0.02 1 116 . 27 THR HA H 4.57 0.02 1 117 . 27 THR HB H 4.13 0.02 1 118 . 28 LYS HA H 4.38 0.02 1 119 . 28 LYS HB2 H 1.78 0.02 2 120 . 28 LYS HB3 H 1.70 0.02 2 121 . 28 LYS HG2 H 1.40 0.02 1 122 . 28 LYS HD2 H 1.63 0.02 1 123 . 28 LYS HE2 H 2.90 0.02 1 124 . 29 PRO HA H 4.46 0.02 1 125 . 29 PRO HB2 H 2.27 0.02 2 126 . 29 PRO HB3 H 2.00 0.02 2 127 . 29 PRO HG2 H 1.96 0.02 1 128 . 29 PRO HD2 H 3.66 0.02 2 129 . 29 PRO HD3 H 3.54 0.02 2 130 . 30 THR H H 7.73 0.02 1 131 . 30 THR HA H 4.12 0.02 1 132 . 30 THR HB H 4.22 0.02 1 133 . 30 THR HG2 H 1.19 0.02 1 stop_ save_