data_15641 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H-NMR Chemical shifts and vicinal coupling constants (3JHNHa) for 24-residue peptide corresponding to the segment within ice nucleation protein of Erwinia uredovora, Erwinia herbicola ; _BMRB_accession_number 15641 _BMRB_flat_file_name bmr15641.str _Entry_type new _Submission_date 2008-01-25 _Accession_date 2008-01-25 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Kumaki Yasuhiro . . 2 Kawano Keiichi . . 3 Hikichi Kunio . . 4 Matsumoto Takeshi . . 5 Matsushima Norio . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 coupling_constants 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 121 "coupling constants" 12 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2008-05-28 original author . stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_title 'A circular loop of the sixteen-residue repeating unit in ice nucleation protein' _Citation_status published _Citation_type journal _PubMed_ID 18361918 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Kumaki Yasuhiro . . 2 Kawano Keiichi . . 3 Hikichi Kunio . . 4 Matsumoto Takeshi . . 5 Matsushima Norio . . stop_ _Journal_abbreviation 'Biochem. Biophys. Res. Commun.' _Journal_volume 371 _Journal_issue 1 _Page_first 5 _Page_last 9 _Year 2008 loop_ _Keyword 'ice nucleation protein' 'tandem repeat' 'circular loop' 'aromatic ring interaction' stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name monomer loop_ _Mol_system_component_name _Mol_label 'polymer chains' $model_peptide_for_INP stop_ _System_physical_state native _System_oligomer_state ? _System_paramagnetic no save_ ######################## # Monomeric polymers # ######################## save_model_peptide_for_INP _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common model_peptide_for_INP _Mol_thiol_state 'not present' ############################## # Polymer residue sequence # ############################## _Residue_count 24 _Mol_residue_sequence ; SGLRSVLTAGYGSSLISGRR SSLT ; loop_ _Residue_seq_code _Residue_label 1 SER 2 GLY 3 LEU 4 ARG 5 SER 6 VAL 7 LEU 8 THR 9 ALA 10 GLY 11 TYR 12 GLY 13 SER 14 SER 15 LEU 16 ILE 17 SER 18 GLY 19 ARG 20 ARG 21 SER 22 SER 23 LEU 24 THR stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $model_peptide_for_INP 'Erwinia herbicola' 553 Bacteria . Pantoea ananatis 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 $model_peptide_for_INP 'chemical synthesis' . . . . ? stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $model_peptide_for_INP 6 mM 'natural abundance' 'acetic acid' 50 mM 'natural abundance' TSP 1 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_DELTA _Saveframe_category software _Name DELTA _Version 4.3.2 loop_ _Vendor _Address _Electronic_address JEOL . . stop_ loop_ _Task processing stop_ save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer JEOL _Model ALPHA _Field_strength 500 save_ ############################# # NMR applied experiments # ############################# save_2D_DQF-COSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _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_NOESY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units temperature 278 . K pH 4.0 . pH pressure 1 . atm 'ionic strength' 0.05 . M stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference_1 _Saveframe_category chemical_shift_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 TSP H 1 'methyl protons' ppm 0.0 internal direct ? ? ? 1 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # The values other than 1 are used for those atoms with different # # chemical shifts that cannot be assigned to stereospecific atoms # # or to specific residues or chains. # # # # Index Value Definition # # # # 1 Unique (including isolated methyl protons, # # geminal atoms, and geminal methyl # # groups with identical chemical shifts) # # (e.g. ILE HD11, HD12, HD13 protons) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups (e.g. ASP HB2 and HB3 # # protons, LEU CD1 and CD2 carbons, or # # LEU HD11, HD12, HD13 and HD21, HD22, # # HD23 methyl protons) # # 3 Aromatic atoms on opposite sides of # # symmetrical rings (e.g. TYR HE1 and HE2 # # protons) # # 4 Intraresidue ambiguities (e.g. LYS HG and # # HD protons or TRP HZ2 and HZ3 protons) # # 5 Interresidue ambiguities (LYS 12 vs. LYS 27) # # 6 Intermolecular ambiguities (e.g. ASP 31 CA # # in monomer 1 and ASP 31 CA in monomer 2 # # of an asymmetrical homodimer, duplex # # DNA assignments, or other assignments # # that may apply to atoms in one or more # # molecule in the molecular assembly) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_assigned_chem_shift_list_1 _Saveframe_category assigned_chemical_shifts loop_ _Software_label $DELTA stop_ loop_ _Experiment_label '2D DQF-COSY' '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 'polymer chains' 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 SER HA H 4.22 0.02 1 2 1 1 SER HB2 H 4.03 0.02 1 3 1 1 SER HB3 H 4.03 0.02 1 4 2 2 GLY H H 8.83 0.02 1 5 2 2 GLY HA2 H 4.03 0.02 1 6 2 2 GLY HA3 H 4.03 0.02 1 7 3 3 LEU H H 8.44 0.02 1 8 3 3 LEU HA H 4.34 0.02 1 9 3 3 LEU HB2 H 1.61 0.02 1 10 3 3 LEU HB3 H 1.61 0.02 1 11 3 3 LEU HD1 H 0.89 0.02 2 12 3 3 LEU HD2 H 0.93 0.02 2 13 3 3 LEU HG H 1.61 0.02 1 14 4 4 ARG H H 8.58 0.02 1 15 4 4 ARG HA H 4.36 0.02 1 16 4 4 ARG HB2 H 1.78 0.02 2 17 4 4 ARG HB3 H 1.84 0.02 2 18 4 4 ARG HD2 H 3.19 0.02 1 19 4 4 ARG HD3 H 3.19 0.02 1 20 4 4 ARG HE H 7.24 0.02 1 21 4 4 ARG HG2 H 1.65 0.02 1 22 4 4 ARG HG3 H 1.65 0.02 1 23 5 5 SER H H 8.46 0.02 1 24 5 5 SER HA H 4.47 0.02 1 25 5 5 SER HB2 H 3.85 0.02 1 26 5 5 SER HB3 H 3.85 0.02 1 27 6 6 VAL H H 8.33 0.02 1 28 6 6 VAL HA H 4.12 0.02 1 29 6 6 VAL HB H 2.09 0.02 1 30 6 6 VAL HG1 H 0.93 0.02 1 31 6 6 VAL HG2 H 0.93 0.02 1 32 7 7 LEU H H 8.41 0.02 1 33 7 7 LEU HA H 4.41 0.02 1 34 7 7 LEU HB2 H 1.63 0.02 4 35 7 7 LEU HB3 H 1.63 0.02 4 36 7 7 LEU HD1 H 0.83 0.02 2 37 7 7 LEU HD2 H 0.9 0.02 2 38 7 7 LEU HG H 1.58 0.02 4 39 8 8 THR H H 8.15 0.02 1 40 8 8 THR HA H 4.29 0.02 1 41 8 8 THR HB H 4.21 0.02 1 42 8 8 THR HG2 H 1.2 0.02 1 43 9 9 ALA H H 8.43 0.02 1 44 9 9 ALA HA H 4.3 0.02 1 45 9 9 ALA HB H 1.38 0.02 1 46 10 10 GLY H H 8.46 0.02 1 47 10 10 GLY HA2 H 3.9 0.02 2 48 10 10 GLY HA3 H 3.93 0.02 2 49 11 11 TYR H H 8.23 0.02 1 50 11 11 TYR HA H 4.51 0.02 1 51 11 11 TYR HB2 H 3.01 0.02 2 52 11 11 TYR HB3 H 3.06 0.02 2 53 11 11 TYR HD1 H 7.12 0.02 1 54 11 11 TYR HD2 H 7.12 0.02 1 55 11 11 TYR HE1 H 6.83 0.02 1 56 11 11 TYR HE2 H 6.83 0.02 1 57 12 12 GLY H H 8.57 0.02 1 58 12 12 GLY HA2 H 3.84 0.02 2 59 12 12 GLY HA3 H 3.97 0.02 2 60 13 13 SER H H 8.28 0.02 1 61 13 13 SER HA H 4.47 0.02 1 62 13 13 SER HB2 H 3.86 0.02 2 63 13 13 SER HB3 H 3.92 0.02 2 64 14 14 SER H H 8.5 0.02 1 65 14 14 SER HA H 4.46 0.02 1 66 15 15 LEU H H 8.31 0.02 1 67 15 15 LEU HA H 4.34 0.02 1 68 15 15 LEU HB2 H 1.65 0.02 4 69 15 15 LEU HB3 H 1.65 0.02 4 70 15 15 LEU HD1 H 0.83 0.02 2 71 15 15 LEU HD2 H 0.9 0.02 2 72 15 15 LEU HG H 1.58 0.02 4 73 16 16 ILE H H 8.16 0.02 1 74 16 16 ILE HA H 4.17 0.02 1 75 16 16 ILE HB H 1.88 0.02 1 76 16 16 ILE HD1 H 0.83 0.02 4 77 16 16 ILE HG12 H 1.18 0.02 2 78 16 16 ILE HG13 H 1.46 0.02 2 79 16 16 ILE HG2 H 0.9 0.02 4 80 17 17 SER H H 8.44 0.02 1 81 17 17 SER HA H 4.41 0.02 1 82 17 17 SER HB2 H 3.87 0.02 1 83 17 17 SER HB3 H 3.87 0.02 1 84 18 18 GLY H H 8.49 0.02 1 85 18 18 GLY HA2 H 3.98 0.02 1 86 18 18 GLY HA3 H 3.98 0.02 1 87 19 19 ARG H H 8.19 0.02 1 88 19 19 ARG HA H 4.34 0.02 1 89 19 19 ARG HB2 H 1.76 0.02 2 90 19 19 ARG HB3 H 1.84 0.02 2 91 19 19 ARG HD2 H 3.19 0.02 1 92 19 19 ARG HD3 H 3.19 0.02 1 93 19 19 ARG HE H 7.24 0.02 1 94 19 19 ARG HG2 H 1.63 0.02 1 95 19 19 ARG HG3 H 1.63 0.02 1 96 20 20 ARG H H 8.61 0.02 1 97 20 20 ARG HA H 4.38 0.02 1 98 20 20 ARG HB2 H 1.79 0.02 2 99 20 20 ARG HB3 H 1.88 0.02 2 100 20 20 ARG HD2 H 3.2 0.02 1 101 20 20 ARG HD3 H 3.2 0.02 1 102 20 20 ARG HE H 7.24 0.02 1 103 20 20 ARG HG2 H 1.67 0.02 1 104 20 20 ARG HG3 H 1.67 0.02 1 105 21 21 SER H H 8.56 0.02 1 106 21 21 SER HA H 4.47 0.02 1 107 22 22 SER H H 8.48 0.02 1 108 22 22 SER HA H 4.5 0.02 1 109 22 22 SER HB2 H 3.88 0.02 1 110 22 22 SER HB3 H 3.88 0.02 1 111 23 23 LEU H H 8.48 0.02 1 112 23 23 LEU HA H 4.42 0.02 1 113 23 23 LEU HB2 H 1.66 0.02 1 114 23 23 LEU HB3 H 1.66 0.02 1 115 23 23 LEU HD1 H 0.87 0.02 2 116 23 23 LEU HD2 H 0.94 0.02 2 117 23 23 LEU HG H 1.66 0.02 1 118 24 24 THR H H 7.82 0.02 1 119 24 24 THR HA H 4.26 0.02 1 120 24 24 THR HB H 4.19 0.02 1 121 24 24 THR HG2 H 1.15 0.02 1 stop_ loop_ _Atom_shift_assign_ID_ambiguity 34 '35,38' '68,69,72' '76,76,76,79,79,79' stop_ save_ ######################## # Coupling constants # ######################## save_coupling_constant_list_1 _Saveframe_category coupling_constants loop_ _Software_label $DELTA stop_ loop_ _Experiment_label '2D DQF-COSY' stop_ _Sample_conditions_label $sample_conditions_1 _Spectrometer_frequency_1H 500 _Mol_system_component_name 'polymer chains' loop_ _Coupling_constant_ID _Coupling_constant_code _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_name _Coupling_constant_value _Coupling_constant_min_value _Coupling_constant_max_value _Coupling_constant_value_error 1 3JHNHA 4 ARG H 4 ARG HA 6.5 . . 1.5 2 3JHNHA 6 VAL H 6 VAL HA 7.8 . . 1.5 3 3JHNHA 8 THR H 8 THR HA 6.9 . . 1.5 4 3JHNHA 11 TYR H 11 TYR HA 6.9 . . 1.5 5 3JHNHA 13 SER H 13 SER HA 5.4 . . 1.5 6 3JHNHA 15 LEU H 15 LEU HA 6.9 . . 1.5 7 3JHNHA 16 ILE H 16 ILE HA 7.5 . . 1.5 8 3JHNHA 19 ARG H 19 ARG HA 6.5 . . 1.5 9 3JHNHA 20 ARG H 20 ARG HA 6.9 . . 1.5 10 3JHNHA 21 SER H 21 SER HA 6.7 . . 1.5 11 3JHNHA 22 SER H 22 SER HA 6.9 . . 1.5 12 3JHNHA 24 THR H 24 THR HA 8.8 . . 1.5 stop_ save_