data_6857 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Solution structure of an immunodominant epitope of myelin basic protein (MBP) - Conformational dependence on environment of an intrinsically unstructured protein ; _BMRB_accession_number 6857 _BMRB_flat_file_name bmr6857.str _Entry_type original _Submission_date 2005-10-09 _Accession_date 2005-10-10 _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 Fares Christophe . . 2 Libich David S. . 3 Harauz George . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 3 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 327 "13C chemical shifts" 84 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2006-04-20 original author . stop_ _Original_release_date 2006-04-20 save_ ############################# # Citation for this entry # ############################# save_Primary_Citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Solution NMR structure of an immunodominant epitope of myelin basic protein' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 16420483 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Fares Christophe . . 2 Libich David S. . 3 Harauz George . . stop_ _Journal_abbreviation 'FEBS J.' _Journal_volume 273 _Journal_issue 3 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 601 _Page_last 614 _Year 2006 _Details . loop_ _Keyword 'amphipathic helix' 'correlation spectroscopy' 'immunodominant epitope' 'multiple sclerosis' 'myelin basic protein' 'solution NMR' stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'FF2 immunodominant peptide' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label FF2 $MBP_immunodominant_polypeptide stop_ _System_molecular_weight 2141.4 _System_physical_state native _System_oligomer_state protein _System_paramagnetic no _System_thiol_state 'not present' loop_ _Biological_function 'imunodominant epitope of mylin basic protein' stop_ _Database_query_date . _Details ; an 18mer peptide derived from the immunodominat epitope (81-98, human numbering) of myelin basic protein ; save_ ######################## # Monomeric polymers # ######################## save_MBP_immunodominant_polypeptide _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common FF2 _Molecular_mass 2141.4 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 18 _Mol_residue_sequence QDENPVVHFFKNIVTPRT loop_ _Residue_seq_code _Residue_label 1 GLN 2 ASP 3 GLU 4 ASN 5 PRO 6 VAL 7 VAL 8 HIS 9 PHE 10 PHE 11 LYS 12 ASN 13 ILE 14 VAL 15 THR 16 PRO 17 ARG 18 THR 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 15131 MBP 100.00 176 100.00 100.00 6.14e-04 BMRB 18520 "S72-S107 peptide of 18.5kDa murine MBP" 100.00 36 100.00 100.00 1.98e-03 BMRB 19186 S72-S107 100.00 36 100.00 100.00 1.98e-03 BMRB 20062 Myelin_Basic_Protein 88.89 17 100.00 100.00 2.33e-01 BMRB 6100 rmMBP 100.00 176 100.00 100.00 6.14e-04 PDB 1BX2 "Crystal Structure Of Hla-Dr2 (Dra0101,Drb11501) Complexed With A Peptide From Human Myelin Basic Protein" 83.33 15 100.00 100.00 9.04e-01 PDB 1FV1 "Structural Basis For The Binding Of An Immunodominant Peptide From Myelin Basic Protein In Different Registers By Two Hla-Dr2 A" 83.33 20 100.00 100.00 1.16e+00 PDB 1YMM "TcrHLA-Dr2bMBP-Peptide Complex" 83.33 23 100.00 100.00 8.05e-01 PDB 2LUG "Solution Nmr Structure Of A S72-s107 Peptide Of 18.5kda Murine Myelin Basic Protein (mbp) In Association With Dodecylphosphocho" 100.00 36 100.00 100.00 1.98e-03 PDB 3PL6 "Structure Of Autoimmune Tcr Hy.1b11 In Complex With Hla-Dq1 And Mbp 85-99" 83.33 268 100.00 100.00 8.11e-01 DBJ BAB23830 "unnamed protein product [Mus musculus]" 100.00 128 100.00 100.00 1.13e-03 DBJ BAC37705 "unnamed protein product [Mus musculus]" 100.00 154 100.00 100.00 1.61e-03 DBJ BAE28256 "unnamed protein product [Mus musculus]" 100.00 128 100.00 100.00 1.13e-03 DBJ BAE87162 "unnamed protein product [Macaca fascicularis]" 100.00 160 100.00 100.00 3.93e-04 DBJ BAE87443 "unnamed protein product [Macaca fascicularis]" 100.00 140 100.00 100.00 2.12e-03 EMBL CAA10804 "myelin basic protein [Rattus norvegicus]" 100.00 128 100.00 100.00 1.22e-03 EMBL CAA10805 "myelin basic protein [Rattus norvegicus]" 100.00 154 100.00 100.00 1.70e-03 EMBL CAA10806 "myelin basic protein [Rattus norvegicus]" 100.00 169 100.00 100.00 2.55e-04 EMBL CAA10807 "myelin basic protein [Rattus norvegicus]" 100.00 195 100.00 100.00 5.58e-04 EMBL CAA35179 "myelin basic protein [Homo sapiens]" 100.00 197 100.00 100.00 6.64e-04 GB AAA37720 "alternate [Mus musculus]" 100.00 250 100.00 100.00 5.72e-03 GB AAA39496 "18.5 kd myelin basic protein, partial [Mus musculus]" 100.00 169 100.00 100.00 2.47e-04 GB AAA39497 "14 kd myelin basic protein, partial [Mus musculus]" 100.00 128 100.00 100.00 1.13e-03 GB AAA39499 "14 kd myelin basic protein [Mus musculus]" 100.00 128 100.00 100.00 1.13e-03 GB AAA39500 "17 kd myelin basic protein [Mus musculus]" 100.00 154 100.00 100.00 1.61e-03 PRF 0411226A "fibroblast growth factor G 44-166" 100.00 123 100.00 100.00 1.62e-04 PRF 1003243A "protein 21.5K,myelin basic" 100.00 199 100.00 100.00 2.92e-04 PRF 1102236A "protein,myelin basic" 100.00 172 100.00 100.00 3.29e-04 REF NP_001001546 "myelin basic protein [Sus scrofa]" 100.00 173 100.00 100.00 3.14e-04 REF NP_001020252 "myelin basic protein isoform 1 [Homo sapiens]" 100.00 197 100.00 100.00 6.64e-04 REF NP_001020261 "myelin basic protein isoform 3 [Homo sapiens]" 100.00 171 100.00 100.00 2.68e-04 REF NP_001020263 "myelin basic protein isoform 4 [Homo sapiens]" 100.00 160 100.00 100.00 5.16e-04 REF NP_001020272 "Golli-MBP isoform 1 [Homo sapiens]" 100.00 304 100.00 100.00 2.60e-03 SP P02686 "RecName: Full=Myelin basic protein; Short=MBP; AltName: Full=Myelin A1 protein; AltName: Full=Myelin membrane encephalitogenic " 100.00 304 100.00 100.00 2.60e-03 SP P02687 "RecName: Full=Myelin basic protein; Short=MBP; AltName: Full=20 kDa microtubule-stabilizing protein; AltName: Full=Myelin A1 pr" 100.00 169 100.00 100.00 1.94e-04 SP P02688 "RecName: Full=Myelin basic protein; Short=MBP [Rattus norvegicus]" 100.00 195 100.00 100.00 5.03e-04 SP P04370 "RecName: Full=Myelin basic protein; Short=MBP; AltName: Full=Myelin A1 protein [Mus musculus]" 100.00 250 100.00 100.00 5.72e-03 SP P06906 "RecName: Full=Myelin basic protein; Short=MBP [Pan troglodytes]" 100.00 171 100.00 100.00 2.60e-04 TPG DAA16031 "TPA: myelin basic protein [Bos taurus]" 100.00 329 100.00 100.00 3.25e-03 stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $MBP_immunodominant_polypeptide Mouse 10090 Eukaryota Metazoa Mus musculus 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 $MBP_immunodominant_polypeptide 'chemical synthesis' . . . . . 'synthesised using F-moc peptide chemistry' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details 'FF2 in aqueous solution' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $MBP_immunodominant_polypeptide 2 mM no KCl 100 mM no stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details 'FF2 in organic solution' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $MBP_immunodominant_polypeptide 5 mM . TFE 30 % [U-2H] stop_ save_ save_sample_3 _Saveframe_category sample _Sample_type micelle _Details 'FF2 in micelles' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $MBP_immunodominant_polypeptide 1 mM . DPC 100 mM [U-2H] stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name XWINNMR _Version 3.5 loop_ _Vendor _Address _Electronic_address Bruker 'Milton, Ontario, Canada' http://www.bruker.ca stop_ loop_ _Task processing stop_ _Details . save_ save_software_2 _Saveframe_category software _Name SPARKY _Version 3.111 loop_ _Vendor _Address _Electronic_address 'UCSF NMR Lab' . http://www.cgl.ucsf.edu/home/sparky/ stop_ loop_ _Task assignment stop_ _Details 'T. D. Goddard and D. G. Kneller, SPARKY 3, University of California, San Francisco.' save_ save_software_3 _Saveframe_category software _Name ARIA _Version 2.0 loop_ _Vendor _Address _Electronic_address 'Jens Linge, Michael Nilges' . http://www.pasteur.fr/recherche/unites/Binfs/aria/ stop_ loop_ _Task 'Structure calculation/refinement' stop_ _Details 'JP Linge, SI O'Donoghue and M Nilges. Assigning Ambiguous NOEs with ARIA. Methods in Enzymology (2001), 339, 71-90.' save_ save_software_4 _Saveframe_category software _Name CNS _Version 2.0 loop_ _Vendor _Address _Electronic_address 'Jens Linge, Michael Nilges' . http://www.pasteur.fr/recherche/unites/Binfs/aria/ stop_ loop_ _Task 'Structure calculation/refinement' stop_ _Details 'JP Linge, SI O'Donoghue and M Nilges. Assigning Ambiguous NOEs with ARIA. Methods in Enzymology (2001), 339, 71-90.' save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_Spectrometer _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D-TOCSY_(using_DIPSI-2)_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D-TOCSY (using DIPSI-2)' _Sample_label . save_ save_2D-NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name 2D-NOESY _Sample_label . save_ save_1H-13C_HSQC_(natural_abundance)_3 _Saveframe_category NMR_applied_experiment _Experiment_name '1H-13C HSQC (natural abundance)' _Sample_label . save_ save_2D-TOCSY_(using_DIPSI-2) _Saveframe_category NMR_applied_experiment _Experiment_name '2D-TOCSY (using DIPSI-2)' _BMRB_pulse_sequence_accession_number . _Details . save_ save_2D-NOESY _Saveframe_category NMR_applied_experiment _Experiment_name 2D-NOESY _BMRB_pulse_sequence_accession_number . _Details . save_ save_1H-13C_HSQC_(natural_abundance) _Saveframe_category NMR_applied_experiment _Experiment_name '1H-13C HSQC (natural abundance)' _BMRB_pulse_sequence_accession_number . _Details . save_ ####################### # Sample conditions # ####################### save_conditions_1 _Saveframe_category sample_conditions _Details 'conditions of FF2 in KCl' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 6.5 0.1 pH temperature 298 0.1 K stop_ save_ save_conditions_2 _Saveframe_category sample_conditions _Details 'conditions of FF2 in TFE' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 6.5 0.1 pH temperature 300 0.1 K stop_ save_ save_conditions_3 _Saveframe_category sample_conditions _Details 'conditions of FF2 in DPC' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 6.5 0.1 pH temperature 318 0.1 K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_referencing _Saveframe_category chemical_shift_reference _Details ; The 13C chemical shifts were referenced indiretly to TPS using the shift ratio 0.25144954. ; 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 TPS C 13 'methyl protons' ppm 0 external indirect . 'outside sample' . 0.25144954 TPS H 1 'methyl protons' ppm 0 external indirect . 'outside sample' . 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_chem_shift_list_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_2 stop_ loop_ _Experiment_label '2D-TOCSY (using DIPSI-2)' '1H-13C HSQC (natural abundance)' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $conditions_1 _Chem_shift_reference_set_label $chemical_shift_referencing _Mol_system_component_name FF2 _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 GLN HA H 4.126 0.003 1 2 1 1 GLN HB2 H 2.211 0.008 2 3 1 1 GLN HG2 H 2.464 0.006 2 4 1 1 GLN CA C 55.355 0.001 1 5 1 1 GLN CB C 29.366 0.001 1 6 1 1 GLN CG C 32.108 0.001 1 7 2 2 ASP H H 8.988 0.136 1 8 2 2 ASP HA H 4.764 0.035 1 9 2 2 ASP HB2 H 2.976 0.011 1 10 2 2 ASP HB3 H 2.893 0.004 1 11 2 2 ASP CA C 53.165 0.001 1 12 2 2 ASP CB C 38.234 0.001 1 13 3 3 GLU H H 8.592 0.020 1 14 3 3 GLU HA H 4.435 0.006 1 15 3 3 GLU HB2 H 2.155 0.006 1 16 3 3 GLU HB3 H 1.987 0.003 1 17 3 3 GLU HG2 H 2.487 0.005 1 18 3 3 GLU CA C 56.005 0.001 1 19 3 3 GLU CB C 28.906 0.046 1 20 3 3 GLU CG C 32.746 0.001 1 21 4 4 ASN H H 8.443 0.019 1 22 4 4 ASN HA H 4.998 0.003 1 23 4 4 ASN HB2 H 2.851 0.003 1 24 4 4 ASN HB3 H 2.714 0.007 1 25 4 4 ASN CA C 51.577 0.001 1 26 4 4 ASN CB C 38.923 0.001 1 27 5 5 PRO HA H 4.468 0.010 1 28 5 5 PRO HB2 H 2.330 0.001 1 29 5 5 PRO HB3 H 2.293 0.005 1 30 5 5 PRO HG2 H 2.033 0.008 1 31 5 5 PRO HG3 H 1.943 0.034 1 32 5 5 PRO HD2 H 3.817 0.035 1 33 5 5 PRO HD3 H 3.746 0.008 1 34 5 5 PRO CA C 63.465 0.001 1 35 5 5 PRO CB C 32.272 0.001 1 36 5 5 PRO CG C 27.412 0.001 1 37 5 5 PRO CD C 50.929 0.147 1 38 6 6 VAL H H 8.165 0.022 1 39 6 6 VAL HA H 4.037 0.021 1 40 6 6 VAL HB H 1.960 0.048 1 41 6 6 VAL HG1 H 0.809 0.074 2 42 6 6 VAL HG2 H 0.885 0.043 2 43 6 6 VAL CA C 62.458 0.001 1 44 6 6 VAL CB C 32.657 0.001 1 45 6 6 VAL CG1 C 20.707 0.001 1 46 6 6 VAL CG2 C 20.823 0.001 1 47 7 7 VAL H H 8.061 0.022 1 48 7 7 VAL HA H 4.029 0.008 1 49 7 7 VAL HB H 1.925 0.007 1 50 7 7 VAL HG1 H 0.760 0.004 2 51 7 7 VAL HG2 H 0.877 0.014 2 52 7 7 VAL CA C 62.297 0.001 1 53 7 7 VAL CB C 30.903 0.001 1 54 7 7 VAL CG1 C 21.058 0.001 1 55 7 7 VAL CG2 C 17.630 0.001 1 56 8 8 HIS H H 8.273 0.001 1 57 8 8 HIS HA H 4.668 0.017 1 58 8 8 HIS HB2 H 3.067 0.004 1 59 8 8 HIS HB3 H 3.067 0.004 1 60 8 8 HIS HD2 H 7.220 0.007 1 61 8 8 HIS HE1 H 8.628 0.004 1 62 8 8 HIS CA C 54.719 0.001 1 63 8 8 HIS CB C 29.471 0.001 1 64 8 8 HIS CD2 C 120.110 0.001 1 65 8 8 HIS CE1 C 136.418 0.001 1 66 8 8 HIS HD1 H 8.474 0.013 1 67 9 9 PHE H H 8.305 0.029 1 68 9 9 PHE HA H 4.612 0.088 1 69 9 9 PHE HB2 H 3.019 0.006 1 70 9 9 PHE HB3 H 2.932 0.015 1 71 9 9 PHE HD1 H 7.208 0.011 1 72 9 9 PHE HD2 H 7.208 0.011 1 73 9 9 PHE HE1 H 7.072 0.006 1 74 9 9 PHE HE2 H 7.072 0.006 1 75 9 9 PHE CA C 57.724 0.001 1 76 9 9 PHE CB C 38.213 0.013 1 77 9 9 PHE CD1 C 133.584 0.001 1 78 9 9 PHE CD2 C 133.584 0.001 1 79 9 9 PHE CE1 C 118.247 0.001 1 80 9 9 PHE CE2 C 118.247 0.001 1 81 10 10 PHE H H 8.295 0.015 1 82 10 10 PHE HA H 4.583 0.005 1 83 10 10 PHE HB2 H 3.095 0.004 1 84 10 10 PHE HB3 H 2.956 0.004 1 85 10 10 PHE HD1 H 7.259 0.005 1 86 10 10 PHE HD2 H 7.259 0.005 1 87 10 10 PHE HE1 H 7.093 0.037 1 88 10 10 PHE HE2 H 7.093 0.037 1 89 10 10 PHE CA C 57.521 0.001 1 90 10 10 PHE CB C 39.406 0.037 1 91 10 10 PHE CD1 C 133.854 0.001 1 92 10 10 PHE CD2 C 133.854 0.001 1 93 10 10 PHE CE1 C 118.034 0.001 1 94 10 10 PHE CE2 C 118.034 0.001 1 95 11 11 LYS H H 8.215 0.017 1 96 11 11 LYS HA H 4.239 0.005 1 97 11 11 LYS HB2 H 1.795 0.004 1 98 11 11 LYS HB3 H 1.795 0.004 1 99 11 11 LYS HG2 H 1.395 0.008 1 100 11 11 LYS HG3 H 1.395 0.008 1 101 11 11 LYS HD2 H 1.714 0.006 1 102 11 11 LYS HD3 H 1.714 0.006 1 103 11 11 LYS HE2 H 3.020 0.004 1 104 11 11 LYS HE3 H 3.020 0.004 1 105 11 11 LYS HZ H 7.582 0.019 1 106 11 11 LYS CA C 56.348 0.001 1 107 11 11 LYS CB C 33.476 0.001 1 108 11 11 LYS CG C 24.830 0.001 1 109 11 11 LYS CD C 29.309 0.001 1 110 11 11 LYS CE C 40.793 1.457 1 111 12 12 ASN H H 8.449 0.012 1 112 12 12 ASN HA H 4.691 0.004 1 113 12 12 ASN HB2 H 2.836 0.004 1 114 12 12 ASN HB3 H 2.748 0.013 1 115 12 12 ASN CA C 53.417 0.001 1 116 12 12 ASN CB C 38.943 0.001 1 117 13 13 ILE H H 8.132 0.018 1 118 13 13 ILE HA H 4.227 0.003 1 119 13 13 ILE HB H 1.893 0.006 1 120 13 13 ILE HG12 H 1.195 0.005 1 121 13 13 ILE HG2 H 1.472 0.006 1 122 13 13 ILE HD1 H 0.901 0.007 1 123 13 13 ILE CA C 61.152 0.001 1 124 13 13 ILE CB C 39.018 0.001 1 125 13 13 ILE CG1 C 27.263 0.001 1 126 13 13 ILE CD1 C 13.001 0.001 1 127 14 14 VAL H H 8.275 0.058 1 128 14 14 VAL HA H 4.194 0.040 1 129 14 14 VAL HB H 2.068 0.003 1 130 14 14 VAL HG1 H 0.828 0.034 2 131 14 14 VAL HG2 H 0.938 0.010 2 132 14 14 VAL CA C 62.304 0.001 1 133 14 14 VAL CB C 32.880 0.001 1 134 14 14 VAL CG1 C 21.157 0.037 1 135 15 15 THR H H 8.301 0.019 1 136 15 15 THR HA H 4.625 0.008 1 137 15 15 THR HB H 4.162 0.008 1 138 15 15 THR HG2 H 1.278 0.006 1 139 15 15 THR CA C 59.860 0.001 1 140 15 15 THR CB C 69.845 0.001 1 141 15 15 THR CG2 C 21.520 0.001 1 142 16 16 PRO HA H 4.461 0.005 1 143 16 16 PRO HG2 H 2.083 0.004 1 144 16 16 PRO HG3 H 1.961 0.003 1 145 16 16 PRO HD2 H 3.911 0.004 1 146 16 16 PRO HD3 H 3.762 0.005 1 147 16 16 PRO CA C 63.261 0.001 1 148 16 16 PRO CB C 32.357 0.001 1 149 16 16 PRO CG C 27.665 0.001 1 150 16 16 PRO CD C 51.273 0.001 1 151 17 17 ARG H H 8.486 0.018 1 152 17 17 ARG HA H 4.442 0.009 1 153 17 17 ARG HB2 H 1.934 0.003 1 154 17 17 ARG HB3 H 1.934 0.003 1 155 17 17 ARG HG2 H 1.843 0.006 1 156 17 17 ARG HG3 H 1.743 0.003 1 157 17 17 ARG HE H 7.199 0.009 1 158 17 17 ARG CA C 56.146 0.001 1 159 17 17 ARG CB C 32.393 0.001 1 160 17 17 ARG CG C 30.945 0.001 1 161 17 17 ARG CD C 43.441 0.001 1 162 18 18 THR H H 8.178 0.016 1 163 18 18 THR HA H 4.485 0.004 1 164 18 18 THR HB H 4.426 0.003 1 165 18 18 THR HG2 H 1.221 0.002 1 166 18 18 THR CA C 61.032 0.001 1 167 18 18 THR CB C 70.128 0.001 1 168 18 18 THR CG2 C 21.702 0.001 1 stop_ save_ save_chem_shift_list_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_2 stop_ loop_ _Experiment_label '2D-TOCSY (using DIPSI-2)' '1H-13C HSQC (natural abundance)' stop_ loop_ _Sample_label $sample_2 stop_ _Sample_conditions_label $conditions_2 _Chem_shift_reference_set_label $chemical_shift_referencing _Mol_system_component_name FF2 _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 GLN H H 8.038 0.001 1 2 1 1 GLN HA H 4.443 0.13 1 3 1 1 GLN HB2 H 2.312 0.021 1 4 1 1 GLN HB3 H 2.312 0.001 1 5 1 1 GLN HG2 H 2.766 0.009 1 6 1 1 GLN HG3 H 2.645 0.002 1 7 1 1 GLN CA C 59.2 0.1 1 8 2 2 ASP H H 8.686 0.003 1 9 2 2 ASP HA H 4.932 0.009 1 10 2 2 ASP HB2 H 3.092 0.001 1 11 2 2 ASP HB3 H 3.092 0.001 1 12 2 2 ASP CA C 52.5 0.1 1 13 3 3 GLU H H 8.56 0.001 1 14 3 3 GLU HA H 4.626 0.002 1 15 3 3 GLU HB2 H 2.312 0.002 1 16 3 3 GLU HB3 H 2.163 0.013 1 17 3 3 GLU HG2 H 2.657 0.006 1 18 3 3 GLU HG3 H 2.651 0.001 1 19 3 3 GLU CA C 55.2 0.1 1 20 4 4 ASN H H 8.378 0.001 1 21 4 4 ASN HA H 5.134 0.006 1 22 4 4 ASN HB2 H 3.116 0.003 1 23 4 4 ASN HB3 H 3.122 0.003 1 24 4 4 ASN HD21 H 6.798 0.001 1 25 4 4 ASN HD22 H 7.95 0.001 1 26 4 4 ASN CA C 51.2 0.1 1 27 5 5 PRO HA H 4.597 0.015 1 28 5 5 PRO HB2 H 2.621 0.007 1 29 5 5 PRO HB3 H 2.188 0.005 1 30 5 5 PRO HG2 H 2.306 0.003 1 31 5 5 PRO HG3 H 2.284 0.001 1 32 5 5 PRO HD2 H 4.038 0.008 1 33 5 5 PRO HD3 H 4.15 0.004 1 34 5 5 PRO CA C 64.3 0.1 1 35 6 6 VAL H H 8.11 0.001 1 36 6 6 VAL HA H 4.018 0.006 1 37 6 6 VAL HB H 2.436 0.001 1 38 6 6 VAL HG1 H 1.224 0.005 2 39 6 6 VAL HG2 H 1.238 0.005 2 40 6 6 VAL CA C 64.8 0.1 1 41 7 7 VAL H H 7.8 0.001 1 42 7 7 VAL HA H 3.975 0.011 1 43 7 7 VAL HB H 2.296 0.002 1 44 7 7 VAL HG1 H 1.241 0.008 2 45 7 7 VAL HG2 H 1.189 0.013 2 46 7 7 VAL CA C 64.6 0.1 1 47 8 8 HIS H H 8.299 0.002 1 48 8 8 HIS HA H 4.458 0.002 1 49 8 8 HIS HB2 H 3.479 0.011 1 50 8 8 HIS HB3 H 3.685 0.001 1 51 8 8 HIS HD1 H 7.471 0.002 1 52 8 8 HIS HE1 H 8.825 0.001 1 53 8 8 HIS HE2 H 8.524 0.001 1 54 8 8 HIS CA C 58.3 0.1 1 55 9 9 PHE H H 8.304 0.005 1 56 9 9 PHE HA H 4.455 0.007 1 57 9 9 PHE HB2 H 3.406 0.008 1 58 9 9 PHE HB3 H 3.448 0.009 1 59 9 9 PHE HD1 H 7.112 0.001 3 60 9 9 PHE HD2 H 7.11 0.001 3 61 9 9 PHE HE1 H 7.036 0.002 3 62 9 9 PHE HE2 H 7.03 0.001 3 63 9 9 PHE CA C 60.2 0.1 1 64 10 10 PHE H H 8.524 0.001 1 65 10 10 PHE HA H 4.369 0.01 1 66 10 10 PHE HB2 H 3.355 0.011 1 67 10 10 PHE HB3 H 3.315 0.01 1 68 10 10 PHE HD1 H 7.476 0.002 3 69 10 10 PHE HD2 H 7.472 0.001 3 70 10 10 PHE HE1 H 7.191 0.001 3 71 10 10 PHE HE2 H 7.179 0.01 3 72 10 10 PHE CA C 60.7 0.1 1 73 11 11 LYS H H 8.691 0.001 1 74 11 11 LYS HA H 4.24 0.009 1 75 11 11 LYS HB2 H 2.08 0.003 1 76 11 11 LYS HB3 H 2.06 0.007 1 77 11 11 LYS HG2 H 1.84 0.018 1 78 11 11 LYS HG3 H 1.765 0.001 1 79 11 11 LYS HD2 H 1.62 0.001 1 80 11 11 LYS HD3 H 1.674 0.017 1 81 11 11 LYS HE2 H 3.18 0.001 1 82 11 11 LYS HE3 H 3.165 0.005 1 83 11 11 LYS HZ H 7.823 0.001 1 84 11 11 LYS CA C 57.5 0.1 1 85 12 12 ASN H H 7.993 0.001 1 86 12 12 ASN HA H 4.771 0.006 1 87 12 12 ASN HB2 H 2.914 0.001 1 88 12 12 ASN HB3 H 2.924 0.002 1 89 12 12 ASN HD21 H 7.571 0.001 1 90 12 12 ASN HD22 H 6.919 0.002 1 91 12 12 ASN CA C 53.7 0.1 1 92 13 13 ILE H H 7.829 0.002 1 93 13 13 ILE HA H 4.247 0.004 1 94 13 13 ILE HB H 2.034 0.002 1 95 13 13 ILE HG12 H 1.267 0.007 1 96 13 13 ILE HG13 H 0.979 0.03 1 97 13 13 ILE HG2 H 1.557 0.011 1 98 13 13 ILE HD1 H 0.893 0.007 1 99 13 13 ILE CA C 61.7 0.1 1 100 14 14 VAL H H 7.833 0.001 1 101 14 14 VAL HA H 4.304 0.008 1 102 14 14 VAL HB H 2.326 0.003 1 103 14 14 VAL HG1 H 1.044 0.008 2 104 14 14 VAL HG2 H 1.065 0.007 2 105 14 14 VAL CA C 62 0.1 1 106 15 15 THR H H 7.905 0.012 1 107 15 15 THR HA H 4.743 0.003 1 108 15 15 THR HB H 4.417 0.008 1 109 15 15 THR HG2 H 1.456 0.003 1 110 15 15 THR CA C 59.8 0.1 1 111 16 16 PRO HA H 4.653 0.003 1 112 16 16 PRO HB2 H 2.532 0.002 1 113 16 16 PRO HB3 H 2.139 0.001 1 114 16 16 PRO HG2 H 2.242 0.001 1 115 16 16 PRO HG3 H 2.217 0.003 1 116 16 16 PRO HD2 H 4.068 0.008 1 117 16 16 PRO HD3 H 3.873 0.004 1 118 16 16 PRO CA C 62.7 0.1 1 119 17 17 ARG H H 8.437 0.014 1 120 17 17 ARG HA H 4.663 0.004 1 121 17 17 ARG HB2 H 2.157 0.004 1 122 17 17 ARG HB3 H 2.001 0.003 1 123 17 17 ARG HG2 H 1.944 0.007 1 124 17 17 ARG HG3 H 1.91 0.001 1 125 17 17 ARG HD2 H 3.441 0.008 1 126 17 17 ARG HD3 H 3.43 0.001 1 127 17 17 ARG HE H 7.418 0.001 1 128 17 17 ARG CA C 55.2 0.1 1 129 18 18 THR H H 8.198 0.008 1 130 18 18 THR HA H 4.684 0.001 1 131 18 18 THR HB H 4.63 0.001 1 132 18 18 THR HG2 H 1.419 0.008 1 133 18 18 THR CA C 59.9 0.1 1 stop_ save_ save_chem_shift_list_3 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $software_2 stop_ loop_ _Experiment_label '2D-TOCSY (using DIPSI-2)' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $conditions_3 _Chem_shift_reference_set_label $chemical_shift_referencing _Mol_system_component_name FF2 _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 GLN H H 8.396 0.001 1 2 1 1 GLN HA H 4.341 0.001 1 3 1 1 GLN HB2 H 1.906 0.001 1 4 1 1 GLN HB3 H 1.984 0.016 1 5 1 1 GLN HG2 H 2.26 0.003 1 6 1 1 GLN HG3 H 2.26 0.003 1 7 2 2 ASP H H 8.797 0.007 1 8 2 2 ASP HA H 4.909 0.005 1 9 2 2 ASP HB2 H 2.786 0.004 1 10 2 2 ASP HB3 H 2.976 0.071 1 11 3 3 GLU H H 8.344 0.005 1 12 3 3 GLU HA H 4.335 0.009 1 13 3 3 GLU HB2 H 1.906 0.014 1 14 3 3 GLU HB3 H 1.972 0.017 1 15 3 3 GLU HG2 H 2.243 0.029 1 16 3 3 GLU HG3 H 2.243 0.029 1 17 4 4 ASN H H 8.364 0.003 1 18 4 4 ASN HA H 4.587 0.004 1 19 4 4 ASN HB2 H 2.553 0.004 1 20 4 4 ASN HB3 H 2.662 0.005 1 21 5 5 PRO HA H 4.434 0.005 1 22 5 5 PRO HB2 H 1.903 0.006 1 23 5 5 PRO HB3 H 2.503 0.006 1 24 5 5 PRO HG2 H 2.057 0.006 1 25 5 5 PRO HG3 H 2.175 0.03 1 26 5 5 PRO HD2 H 3.815 0.009 1 27 5 5 PRO HD3 H 3.999 0.006 1 28 6 6 VAL H H 8.262 0.004 1 29 6 6 VAL HA H 3.773 0.004 1 30 6 6 VAL HB H 2.304 0.004 1 31 6 6 VAL HG1 H 1.062 0.011 1 32 6 6 VAL HG2 H 1.062 0.011 1 33 7 7 VAL H H 7.533 0.002 1 34 7 7 VAL HA H 3.646 0.011 1 35 7 7 VAL HB H 2.259 0.01 1 36 7 7 VAL HG1 H 1.026 0.007 2 37 7 7 VAL HG2 H 1.082 0.006 2 38 8 8 HIS H H 7.95 0.002 1 39 8 8 HIS HA H 4.04 0.005 1 40 8 8 HIS HB2 H 3.069 0.018 1 41 8 8 HIS HB3 H 3.124 0.007 1 42 8 8 HIS HD1 H 6.909 0.005 1 43 8 8 HIS HD2 H 7.325 0.008 1 44 8 8 HIS HE1 H 6.918 0.001 1 45 9 9 PHE H H 7.937 0.007 1 46 9 9 PHE HA H 4.161 0.028 1 47 9 9 PHE HB2 H 3.167 0.029 1 48 9 9 PHE HB3 H 3.255 0.028 1 49 9 9 PHE HD1 H 6.761 0.01 1 50 9 9 PHE HD2 H 6.761 0.01 1 51 9 9 PHE HE1 H 6.867 0.006 1 52 9 9 PHE HE2 H 6.867 0.006 1 53 10 10 PHE H H 7.936 0.005 1 54 10 10 PHE HA H 4.183 0.005 1 55 10 10 PHE HB2 H 3.132 0.004 1 56 10 10 PHE HB3 H 3.286 0.002 1 57 10 10 PHE HD1 H 6.75 0.006 1 58 10 10 PHE HD2 H 6.75 0.006 1 59 10 10 PHE HE1 H 6.838 0.051 1 60 10 10 PHE HE2 H 6.838 0.051 1 61 11 11 LYS H H 8.449 0.005 1 62 11 11 LYS HA H 3.906 0.005 1 63 11 11 LYS HB2 H 1.668 0.012 1 64 11 11 LYS HB3 H 1.818 0.005 1 65 11 11 LYS HG2 H 1.379 0.024 1 66 11 11 LYS HG3 H 1.379 0.024 1 67 11 11 LYS HD2 H 1.622 0.016 1 68 11 11 LYS HD3 H 1.622 0.016 1 69 11 11 LYS HE2 H 2.924 0.023 1 70 11 11 LYS HE3 H 2.841 0.017 1 71 12 12 ASN H H 7.64 0.002 1 72 12 12 ASN HA H 4.486 0.003 1 73 12 12 ASN HB2 H 2.577 0.003 1 74 12 12 ASN HB3 H 2.656 0.005 1 75 13 13 ILE H H 7.351 0.003 1 76 13 13 ILE HA H 3.964 0.003 1 77 13 13 ILE HB H 1.792 0.006 1 78 13 13 ILE HG12 H 1.065 0.005 1 79 13 13 ILE HG13 H 1.373 0.004 1 80 13 13 ILE HG2 H 0.792 0.004 1 81 13 13 ILE HD1 H 0.64 0.005 1 82 14 14 VAL H H 7.335 0.004 1 83 14 14 VAL HA H 4.135 0.002 1 84 14 14 VAL HB H 2.17 0.014 1 85 14 14 VAL HG1 H 0.896 0.007 2 86 14 14 VAL HG2 H 0.896 0.007 2 87 15 15 THR H H 7.694 0.002 1 88 15 15 THR HA H 4.511 0.004 1 89 15 15 THR HB H 4.147 0.008 1 90 15 15 THR HG2 H 1.221 0.003 1 91 16 16 PRO HA H 4.458 0.004 1 92 16 16 PRO HB2 H 1.919 0.009 1 93 16 16 PRO HB3 H 2.307 0.003 1 94 16 16 PRO HG2 H 1.957 0.013 1 95 16 16 PRO HG3 H 2.029 0.004 1 96 16 16 PRO HD2 H 3.635 0.009 1 97 16 16 PRO HD3 H 3.774 0.006 1 98 17 17 ARG H H 8.367 0.005 1 99 17 17 ARG HA H 4.401 0.01 1 100 17 17 ARG HB2 H 1.788 0.018 1 101 17 17 ARG HB3 H 1.92 0.007 1 102 17 17 ARG HG2 H 1.683 0.014 1 103 17 17 ARG HG3 H 1.683 0.014 1 104 17 17 ARG HD2 H 3.215 0.004 1 105 17 17 ARG HD3 H 3.215 0.004 1 106 17 17 ARG HE H 7.119 0.001 1 107 18 18 THR H H 7.663 0.003 1 108 18 18 THR HA H 4.138 0.006 1 109 18 18 THR HB H 4.229 0.003 1 110 18 18 THR HG2 H 1.144 0.003 1 stop_ save_