data_5292 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H Chemical Shift Assignments for TC5b ; _BMRB_accession_number 5292 _BMRB_flat_file_name bmr5292.str _Entry_type original _Submission_date 2002-02-15 _Accession_date 2002-02-15 _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 Neidigh Jonathan W. . 2 Fesinmeyer R. Matthew . 3 Andersen Niels H. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 250 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2002-06-13 original author . stop_ _Original_release_date 2002-06-13 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Designing a 20-residue Protein' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code 22028569 _PubMed_ID 11979279 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Neidigh Jonathan W. . 2 Fesinmeyer R. Matthew . 3 Andersen Niels H. . stop_ _Journal_abbreviation 'Nat. Struct. Biol.' _Journal_volume 9 _Journal_issue 6 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 425 _Page_last 430 _Year 2002 _Details 'First linear 20-residue peptide to display protein-like folding behavior.' loop_ _Keyword miniprotein 'ring current shifts' Trp-cage 'two-state folding' stop_ save_ ################################## # Molecular system description # ################################## save_system_TC5b _Saveframe_category molecular_system _Mol_system_name 'Trp-cage Construct 5b' _Abbreviation_common TC5b _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label TC5b $TC5b stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state monomer _System_paramagnetic no _System_thiol_state 'not present' _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_TC5b _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common 'Trp-cage Construct 5b' _Abbreviation_common TC5b _Molecular_mass . _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 20 _Mol_residue_sequence ; NLYIQWLKDGGPSSGRPPPS ; loop_ _Residue_seq_code _Residue_label 1 ASN 2 LEU 3 TYR 4 ILE 5 GLN 6 TRP 7 LEU 8 LYS 9 ASP 10 GLY 11 GLY 12 PRO 13 SER 14 SER 15 GLY 16 ARG 17 PRO 18 PRO 19 PRO 20 SER stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2014-10-26 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 1L2Y "Nmr Structure Of Trp-Cage Miniprotein Construct Tc5b" 100.00 20 100.00 100.00 1.80e-04 stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Details $TC5b . . . . . . 'Not applicable.' 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 $TC5b '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 $TC5b . mM 1.0 1.8 . 'phosphate buffer' 15 mM . . . H2O 100 % . . . stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Concentration_min_value _Concentration_max_value _Isotopic_labeling $TC5b . mM 1.0 1.8 . 'phosphate buffer' 15 mM . . . Trifluoroethanol 30 % . . . H2O 70 % . . . stop_ save_ ############################ # Computer software used # ############################ save_XWinNMR _Saveframe_category software _Name xwinnmr _Version . loop_ _Task 'data collection' stop_ _Details . save_ save_FELIX _Saveframe_category software _Name FELIX _Version 95 loop_ _Task 'manual peak assignment' processing stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model DRX _Field_strength 500 _Details . save_ ############################# # NMR applied experiments # ############################# save_TOCSY_(15-60ms_spinlock)_1 _Saveframe_category NMR_applied_experiment _Experiment_name 'TOCSY (15-60ms spinlock)' _Sample_label . save_ save_NOESY_(60-200ms_mixing_time)_2 _Saveframe_category NMR_applied_experiment _Experiment_name 'NOESY (60-200ms mixing time)' _Sample_label . save_ save_NMR_spec_expt__0_1 _Saveframe_category NMR_applied_experiment _Experiment_name 'TOCSY (15-60ms spinlock)' _BMRB_pulse_sequence_accession_number . _Details . save_ save_NMR_spec_expt__0_2 _Saveframe_category NMR_applied_experiment _Experiment_name 'NOESY (60-200ms mixing time)' _BMRB_pulse_sequence_accession_number . _Details . save_ ####################### # Sample conditions # ####################### save_Aqueous_Buffer _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 7 0.5 n/a temperature 282 2 K stop_ save_ save_TFE _Saveframe_category sample_conditions _Details 'pH was measured prior to TFE addition.' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 7 1.0 n/a temperature 280 2 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 $Aqueous_Buffer _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name TC5b _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 ASN HA H 4.24 0.005 1 2 . 1 ASN HB2 H 3.14 0.005 1 3 . 1 ASN HB3 H 3.14 0.005 1 4 . 1 ASN HD21 H 7.59 0.005 1 5 . 1 ASN HD22 H 6.97 0.005 1 6 . 2 LEU H H 8.625 0.005 1 7 . 2 LEU HA H 4.134 0.005 1 8 . 2 LEU HB2 H 1.799 0.005 1 9 . 2 LEU HB3 H 1.413 0.005 1 10 . 2 LEU HG H 1.778 0.005 1 11 . 2 LEU HD1 H 0.985 0.005 1 12 . 2 LEU HD2 H 0.915 0.005 1 13 . 3 TYR H H 8.989 0.005 1 14 . 3 TYR HA H 4.139 0.005 1 15 . 3 TYR HB2 H 3.090 0.005 1 16 . 3 TYR HB3 H 3.090 0.005 1 17 . 3 TYR HD1 H 7.025 0.005 1 18 . 3 TYR HD2 H 7.025 0.005 1 19 . 3 TYR HE1 H 6.815 0.005 1 20 . 3 TYR HE2 H 6.815 0.005 1 21 . 4 ILE H H 7.873 0.005 1 22 . 4 ILE HA H 3.805 0.005 1 23 . 4 ILE HB H 1.927 0.005 1 24 . 4 ILE HG12 H 1.709 0.005 2 25 . 4 ILE HG13 H 1.378 0.005 2 26 . 4 ILE HG2 H 0.966 0.005 1 27 . 4 ILE HD1 H 0.960 0.005 1 28 . 5 GLN H H 7.906 0.005 1 29 . 5 GLN HA H 3.947 0.005 1 30 . 5 GLN HB2 H 2.162 0.005 2 31 . 5 GLN HB3 H 2.089 0.005 2 32 . 5 GLN HG2 H 2.385 0.005 2 33 . 5 GLN HG3 H 2.356 0.005 2 34 . 5 GLN HE21 H 7.744 0.005 1 35 . 5 GLN HE22 H 7.063 0.005 1 36 . 6 TRP H H 8.093 0.005 1 37 . 6 TRP HA H 4.252 0.005 1 38 . 6 TRP HB2 H 3.149 0.005 2 39 . 6 TRP HB3 H 3.545 0.005 2 40 . 6 TRP HD1 H 7.036 0.005 1 41 . 6 TRP HE1 H 9.731 0.005 1 42 . 6 TRP HE3 H 7.057 0.005 1 43 . 6 TRP HZ2 H 7.224 0.005 1 44 . 6 TRP HZ3 H 7.133 0.005 1 45 . 6 TRP HH2 H 7.224 0.005 1 46 . 7 LEU H H 8.338 0.005 1 47 . 7 LEU HA H 3.468 0.005 1 48 . 7 LEU HB2 H 1.911 0.005 1 49 . 7 LEU HB3 H 1.375 0.005 1 50 . 7 LEU HG H 1.617 0.005 1 51 . 7 LEU HD1 H 0.986 0.005 1 52 . 7 LEU HD2 H 0.898 0.005 1 53 . 8 LYS H H 8.246 0.005 1 54 . 8 LYS HA H 3.963 0.005 1 55 . 8 LYS HB2 H 1.905 0.005 1 56 . 8 LYS HB3 H 1.905 0.005 1 57 . 8 LYS HG2 H 1.544 0.005 2 58 . 8 LYS HG3 H 1.433 0.005 2 59 . 8 LYS HD2 H 1.636 0.005 1 60 . 8 LYS HD3 H 1.636 0.005 1 61 . 8 LYS HE2 H 2.939 0.005 1 62 . 8 LYS HE3 H 2.939 0.005 1 63 . 8 LYS HZ H 7.620 0.005 1 64 . 9 ASP H H 7.991 0.005 1 65 . 9 ASP HA H 4.573 0.005 1 66 . 9 ASP HB2 H 2.988 0.005 1 67 . 9 ASP HB3 H 2.797 0.005 1 68 . 10 GLY H H 7.627 0.005 1 69 . 10 GLY HA2 H 3.504 0.005 1 70 . 10 GLY HA3 H 4.146 0.005 1 71 . 11 GLY H H 8.375 0.005 1 72 . 11 GLY HA2 H 1.048 0.005 1 73 . 11 GLY HA3 H 3.144 0.005 1 74 . 12 PRO HA H 4.598 0.005 1 75 . 12 PRO HB2 H 2.045 0.005 1 76 . 12 PRO HB3 H 2.501 0.005 1 77 . 12 PRO HG2 H 2.051 0.005 1 78 . 12 PRO HG3 H 2.137 0.005 1 79 . 12 PRO HD2 H 3.779 0.005 1 80 . 12 PRO HD3 H 3.428 0.005 1 81 . 13 SER H H 7.811 0.005 1 82 . 13 SER HA H 4.463 0.005 1 83 . 13 SER HB2 H 3.915 0.005 1 84 . 13 SER HB3 H 3.915 0.005 1 85 . 14 SER H H 8.229 0.005 1 86 . 14 SER HA H 4.179 0.005 1 87 . 14 SER HB2 H 3.545 0.005 1 88 . 14 SER HB3 H 3.874 0.005 1 89 . 15 GLY H H 8.013 0.005 1 90 . 15 GLY HA2 H 3.825 0.005 1 91 . 15 GLY HA3 H 4.256 0.005 1 92 . 16 ARG H H 8.145 0.005 1 93 . 16 ARG HA H 4.980 0.005 1 94 . 16 ARG HB2 H 1.852 0.005 2 95 . 16 ARG HB3 H 1.649 0.005 2 96 . 16 ARG HG2 H 1.850 0.005 2 97 . 16 ARG HG3 H 1.762 0.005 2 98 . 16 ARG HD2 H 3.216 0.005 2 99 . 16 ARG HD3 H 3.297 0.005 2 100 . 16 ARG HE H 7.609 0.005 1 101 . 17 PRO HA H 4.728 0.005 1 102 . 17 PRO HB2 H 1.777 0.005 1 103 . 17 PRO HB3 H 2.313 0.005 1 104 . 17 PRO HG2 H 1.997 0.005 1 105 . 17 PRO HG3 H 1.997 0.005 1 106 . 17 PRO HD2 H 3.659 0.005 1 107 . 17 PRO HD3 H 3.861 0.005 1 108 . 18 PRO HA H 2.659 0.005 1 109 . 18 PRO HB2 H 1.366 0.005 1 110 . 18 PRO HB3 H 0.474 0.005 1 111 . 18 PRO HG2 H 1.751 0.005 1 112 . 18 PRO HG3 H 1.700 0.005 1 113 . 18 PRO HD2 H 3.525 0.005 1 114 . 18 PRO HD3 H 3.516 0.005 1 115 . 19 PRO HA H 4.366 0.005 1 116 . 19 PRO HB2 H 1.973 0.005 1 117 . 19 PRO HB3 H 2.235 0.005 1 118 . 19 PRO HG2 H 1.820 0.005 1 119 . 19 PRO HG3 H 1.847 0.005 1 120 . 19 PRO HD2 H 2.986 0.005 1 121 . 19 PRO HD3 H 3.191 0.005 1 122 . 20 SER H H 8.078 0.005 1 123 . 20 SER HA H 4.230 0.005 1 124 . 20 SER HB2 H 3.808 0.005 1 125 . 20 SER HB3 H 3.808 0.005 1 stop_ save_ save_shift_set_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Sample_label $sample_2 stop_ _Sample_conditions_label $TFE _Chem_shift_reference_set_label $chemical_shift_reference _Mol_system_component_name TC5b _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 ASN HA H 4.18 0.005 1 2 . 1 ASN HB2 H 3.16 0.005 1 3 . 1 ASN HB3 H 3.16 0.005 1 4 . 1 ASN HD21 H 7.45 0.005 1 5 . 1 ASN HD22 H 7.06 0.005 1 6 . 2 LEU H H 8.472 0.005 1 7 . 2 LEU HA H 4.150 0.005 1 8 . 2 LEU HB2 H 1.757 0.005 1 9 . 2 LEU HB3 H 1.506 0.005 1 10 . 2 LEU HG H 1.757 0.005 1 11 . 2 LEU HD1 H 1.003 0.005 2 12 . 2 LEU HD2 H 0.927 0.005 2 13 . 3 TYR H H 8.600 0.005 1 14 . 3 TYR HA H 4.185 0.005 1 15 . 3 TYR HB2 H 3.145 0.005 2 16 . 3 TYR HB3 H 3.032 0.005 2 17 . 3 TYR HD1 H 7.020 0.005 1 18 . 3 TYR HD2 H 7.020 0.005 1 19 . 3 TYR HE1 H 6.805 0.005 1 20 . 3 TYR HE2 H 6.805 0.005 1 21 . 4 ILE H H 7.357 0.005 1 22 . 4 ILE HA H 3.832 0.005 1 23 . 4 ILE HB H 2.062 0.005 1 24 . 4 ILE HG12 H 1.652 0.005 2 25 . 4 ILE HG13 H 1.360 0.005 2 26 . 4 ILE HG2 H 0.990 0.005 1 27 . 4 ILE HD1 H 0.99 0.005 1 28 . 5 GLN H H 7.820 0.005 1 29 . 5 GLN HA H 3.905 0.005 1 30 . 5 GLN HB2 H 2.233 0.005 1 31 . 5 GLN HB3 H 2.233 0.005 1 32 . 5 GLN HG2 H 2.412 0.005 1 33 . 5 GLN HG3 H 2.412 0.005 1 34 . 5 GLN HE21 H 7.447 0.005 1 35 . 5 GLN HE22 H 6.915 0.005 1 36 . 6 TRP H H 8.198 0.005 1 37 . 6 TRP HA H 4.200 0.005 1 38 . 6 TRP HB2 H 3.663 0.005 2 39 . 6 TRP HB3 H 3.168 0.005 2 40 . 6 TRP HD1 H 7.057 0.005 1 41 . 6 TRP HE1 H 9.855 0.005 1 42 . 6 TRP HE3 H 7.269 0.005 1 43 . 6 TRP HZ2 H 7.215 0.005 1 44 . 6 TRP HZ3 H 7.155 0.005 1 45 . 6 TRP HH2 H 7.149 0.005 1 46 . 7 LEU H H 8.391 0.005 1 47 . 7 LEU HA H 3.478 0.005 1 48 . 7 LEU HB2 H 2.136 0.005 1 49 . 7 LEU HB3 H 1.378 0.005 1 50 . 7 LEU HG H 1.882 0.005 1 51 . 7 LEU HD1 H 0.986 0.005 1 52 . 7 LEU HD2 H 0.898 0.005 1 53 . 8 LYS H H 8.762 0.005 1 54 . 8 LYS HA H 3.917 0.005 1 55 . 8 LYS HB2 H 1.950 0.005 1 56 . 8 LYS HB3 H 1.950 0.005 1 57 . 8 LYS HG2 H 1.446 0.005 1 58 . 8 LYS HG3 H 1.446 0.005 1 59 . 8 LYS HD2 H 1.661 0.005 1 60 . 8 LYS HD3 H 1.661 0.005 1 61 . 8 LYS HE2 H 2.933 0.005 1 62 . 8 LYS HE3 H 2.933 0.005 1 63 . 9 ASP H H 7.883 0.005 1 64 . 9 ASP HA H 4.674 0.005 1 65 . 9 ASP HB2 H 3.074 0.005 1 66 . 9 ASP HB3 H 2.946 0.005 1 67 . 10 GLY H H 7.707 0.005 1 68 . 10 GLY HA2 H 3.487 0.005 1 69 . 10 GLY HA3 H 4.211 0.005 1 70 . 11 GLY H H 8.465 0.005 1 71 . 11 GLY HA2 H 0.948 0.005 1 72 . 11 GLY HA3 H 2.880 0.005 1 73 . 12 PRO HA H 4.539 0.005 1 74 . 12 PRO HB2 H 2.075 0.005 1 75 . 12 PRO HB3 H 2.501 0.005 1 76 . 12 PRO HG2 H 2.07 0.005 1 77 . 12 PRO HG3 H 2.16 0.005 1 78 . 12 PRO HD2 H 3.761 0.005 1 79 . 12 PRO HD3 H 3.294 0.005 1 80 . 13 SER H H 7.698 0.005 1 81 . 13 SER HA H 4.424 0.005 1 82 . 13 SER HB2 H 3.954 0.005 1 83 . 13 SER HB3 H 3.954 0.005 1 84 . 14 SER H H 8.162 0.005 1 85 . 14 SER HA H 4.221 0.005 1 86 . 14 SER HB2 H 3.654 0.005 1 87 . 14 SER HB3 H 3.954 0.005 1 88 . 14 SER HG H 4.70 0.005 1 89 . 15 GLY H H 7.905 0.005 1 90 . 15 GLY HA2 H 3.804 0.005 1 91 . 15 GLY HA3 H 4.300 0.005 1 92 . 16 ARG H H 8.141 0.005 1 93 . 16 ARG HA H 5.003 0.005 1 94 . 16 ARG HB2 H 1.956 0.005 2 95 . 16 ARG HB3 H 1.874 0.005 2 96 . 16 ARG HG2 H 1.779 0.005 2 97 . 16 ARG HG3 H 1.741 0.005 2 98 . 16 ARG HD2 H 3.290 0.005 2 99 . 16 ARG HD3 H 3.268 0.005 2 100 . 16 ARG HE H 7.450 0.005 1 101 . 17 PRO HA H 4.671 0.005 1 102 . 17 PRO HB2 H 1.856 0.005 1 103 . 17 PRO HB3 H 2.277 0.005 1 104 . 17 PRO HG2 H 2.014 0.005 1 105 . 17 PRO HG3 H 2.014 0.005 1 106 . 17 PRO HD2 H 3.683 0.005 1 107 . 17 PRO HD3 H 3.884 0.005 1 108 . 18 PRO HA H 2.655 0.005 1 109 . 18 PRO HB2 H 1.329 0.005 1 110 . 18 PRO HB3 H 0.412 0.005 1 111 . 18 PRO HG2 H 1.723 0.005 1 112 . 18 PRO HG3 H 1.494 0.005 1 113 . 18 PRO HD2 H 3.452 0.005 1 114 . 18 PRO HD3 H 3.379 0.005 1 115 . 19 PRO HA H 4.358 0.005 1 116 . 19 PRO HB2 H 1.963 0.005 1 117 . 19 PRO HB3 H 2.170 0.005 1 118 . 19 PRO HG2 H 1.826 0.005 1 119 . 19 PRO HG3 H 1.826 0.005 1 120 . 19 PRO HD2 H 2.922 0.005 1 121 . 19 PRO HD3 H 3.153 0.005 1 122 . 20 SER H H 7.852 0.005 1 123 . 20 SER HA H 4.361 0.005 1 124 . 20 SER HB2 H 3.889 0.005 2 125 . 20 SER HB3 H 3.813 0.005 2 stop_ save_