data_15639 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H-NMR Chemical shifts and vicinal coupling constants (3JHNHa) for 17-residue peptide corresponding to the segment within ice nucleation protein of X. campestris pv. campestris ; _BMRB_accession_number 15639 _BMRB_flat_file_name bmr15639.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" 87 "coupling constants" 10 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 17 _Mol_residue_sequence XTARKGSDLTTGYGSTX loop_ _Residue_seq_code _Residue_label 1 NLQ 2 THR 3 ALA 4 ARG 5 LYS 6 GLY 7 SER 8 ASP 9 LEU 10 THR 11 THR 12 GLY 13 TYR 14 GLY 15 SER 16 THR 17 SET stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2015-06-23 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 20010 model_peptide_for_INP 88.24 19 100.00 100.00 9.09e+00 stop_ save_ ###################### # Polymer residues # ###################### save_chem_comp_NLQ _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common N~2~-ACETYL-L-GLUTAMINE _PDB_code NLQ _Standard_residue_derivative . _Mol_empirical_formula 'C7 H12 N2 O4' _Molecular_mass 188.181 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Tue Aug 21 00:27:49 2007 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons O O O N 0 . ? C C C N 0 . ? OXT OXT O N 0 . ? CA CA C S 0 . ? N N N N 0 . ? C6 C6 C N 0 . ? O4 O4 O N 0 . ? C7 C7 C N 0 . ? CB CB C N 0 . ? CG CG C N 0 . ? CD CD C N 0 . ? NE2 NE2 N N 0 . ? OE1 OE1 O N 0 . ? HO HO H N 0 . ? HA HA H N 0 . ? HN HN H N 0 . ? H71 H71 H N 0 . ? H72 H72 H N 0 . ? H73 H73 H N 0 . ? HB1 HB1 H N 0 . ? HB2 HB2 H N 0 . ? HG1 HG1 H N 0 . ? HG2 HG2 H N 0 . ? HE21 HE21 H N 0 . ? HE22 HE22 H N 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 O C O C SING O HO O HO DOUB C OXT C OXT SING C CA C CA SING CA N CA N SING CA CB CA CB SING CA HA CA HA SING N C6 N C6 SING N HN N HN DOUB C6 O4 C6 O4 SING C6 C7 C6 C7 SING C7 H71 C7 H71 SING C7 H72 C7 H72 SING C7 H73 C7 H73 SING CB CG CB CG SING CB HB1 CB HB1 SING CB HB2 CB HB2 SING CG CD CG CD SING CG HG1 CG HG1 SING CG HG2 CG HG2 SING CD NE2 CD NE2 DOUB CD OE1 CD OE1 SING NE2 HE21 NE2 HE21 SING NE2 HE22 NE2 HE22 stop_ save_ save_chem_comp_SET _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common AMINOSERINE _PDB_code SET _Standard_residue_derivative . _Mol_empirical_formula 'C3 H8 N2 O2' _Molecular_mass 104.108 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Tue Aug 21 02:20:30 2007 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N N 0 . ? CA CA C S 0 . ? CB CB C N 0 . ? OG OG O N 0 . ? NT NT N N 0 . ? C C C N 0 . ? O O O N 0 . ? HN1 HN1 H N 0 . ? HN2 HN2 H N 0 . ? HA HA H N 0 . ? HB1 HB1 H N 0 . ? HB2 HB2 H N 0 . ? HOG HOG H N 0 . ? HNT1 HNT1 H N 0 . ? HNT2 HNT2 H N 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 N CA SING N HN1 N HN1 SING N HN2 N HN2 SING CA CB CA CB SING CA C CA C SING CA HA CA HA SING CB OG CB OG SING CB HB1 CB HB1 SING CB HB2 CB HB2 SING OG HOG OG HOG SING NT C NT C SING NT HNT1 NT HNT1 SING NT HNT2 NT HNT2 DOUB C O C O 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 'Xanthomonas campestris' 339 Bacteria . Xanthomonas campestris 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 3 mM 'natural abundance' DSS 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 4.4 . pH pressure 1 . atm 'ionic strength' 0 . 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 DSS H 1 'methyl protons' ppm 0.00 internal direct ? ? ? 1.000000000 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 NLQ H H 8.52 0.02 1 2 1 1 NLQ HA H 4.34 0.02 1 3 1 1 NLQ HB2 H 1.96 0.02 2 4 1 1 NLQ HB3 H 2.09 0.02 2 5 1 1 NLQ HE21 H 7.68 0.02 1 6 1 1 NLQ HE22 H 7.68 0.02 1 7 1 1 NLQ HG2 H 2.38 0.02 1 8 1 1 NLQ HG3 H 2.38 0.02 1 9 2 2 THR H H 8.43 0.02 1 10 2 2 THR HA H 4.44 0.02 1 11 2 2 THR HB H 4.32 0.02 1 12 2 2 THR HG2 H 1.22 0.02 1 13 3 3 ALA H H 8.46 0.02 1 14 3 3 ALA HA H 4.28 0.02 1 15 3 3 ALA HB H 1.37 0.02 1 16 4 4 ARG H H 8.48 0.02 1 17 4 4 ARG HA H 4.28 0.02 1 18 4 4 ARG HB2 H 1.75 0.02 2 19 4 4 ARG HB3 H 1.8 0.02 2 20 4 4 ARG HD2 H 3.18 0.02 1 21 4 4 ARG HD3 H 3.18 0.02 1 22 4 4 ARG HE H 7.24 0.02 1 23 4 4 ARG HG2 H 1.63 0.02 1 24 4 4 ARG HG3 H 1.63 0.02 1 25 5 5 LYS H H 8.64 0.02 1 26 5 5 LYS HA H 4.32 0.02 1 27 5 5 LYS HB2 H 1.77 0.02 2 28 5 5 LYS HB3 H 1.83 0.02 2 29 5 5 LYS HD2 H 1.67 0.02 1 30 5 5 LYS HD3 H 1.67 0.02 1 31 5 5 LYS HE2 H 3.02 0.02 1 32 5 5 LYS HE3 H 3.02 0.02 1 33 5 5 LYS HG2 H 1.45 0.02 1 34 5 5 LYS HG3 H 1.45 0.02 1 35 5 5 LYS HZ H 7.6 0.02 1 36 6 6 GLY H H 8.69 0.02 1 37 6 6 GLY HA2 H 3.98 0.02 1 38 6 6 GLY HA3 H 3.98 0.02 1 39 7 7 SER H H 8.35 0.02 1 40 7 7 SER HA H 4.42 0.02 1 41 7 7 SER HB2 H 3.86 0.02 1 42 7 7 SER HB3 H 3.86 0.02 1 43 8 8 ASP H H 8.51 0.02 1 44 8 8 ASP HA H 4.61 0.02 1 45 8 8 ASP HB2 H 2.66 0.02 2 46 8 8 ASP HB3 H 2.76 0.02 2 47 9 9 LEU H H 8.36 0.02 1 48 9 9 LEU HA H 4.38 0.02 1 49 9 9 LEU HB2 H 1.68 0.02 4 50 9 9 LEU HB3 H 1.68 0.02 4 51 9 9 LEU HD1 H 0.84 0.02 2 52 9 9 LEU HD2 H 0.91 0.02 2 53 9 9 LEU HG H 1.62 0.02 4 54 10 10 THR H H 8.32 0.02 1 55 10 10 THR HA H 4.37 0.02 1 56 10 10 THR HB H 4.26 0.02 1 57 10 10 THR HG2 H 1.2 0.02 1 58 11 11 THR H H 8.16 0.02 1 59 11 11 THR HA H 4.33 0.02 1 60 11 11 THR HB H 4.2 0.02 1 61 11 11 THR HG2 H 1.18 0.02 1 62 12 12 GLY H H 8.43 0.02 1 63 12 12 GLY HA2 H 3.88 0.02 2 64 12 12 GLY HA3 H 3.94 0.02 2 65 13 13 TYR H H 8.27 0.02 1 66 13 13 TYR HA H 4.53 0.02 1 67 13 13 TYR HB2 H 2.96 0.02 2 68 13 13 TYR HB3 H 3.05 0.02 2 69 13 13 TYR HD1 H 7.11 0.02 1 70 13 13 TYR HD2 H 7.11 0.02 1 71 13 13 TYR HE1 H 6.83 0.02 1 72 13 13 TYR HE2 H 6.83 0.02 1 73 14 14 GLY H H 8.53 0.02 1 74 14 14 GLY HA2 H 3.86 0.02 2 75 14 14 GLY HA3 H 3.94 0.02 2 76 15 15 SER H H 8.3 0.02 1 77 15 15 SER HA H 4.52 0.02 1 78 15 15 SER HB2 H 3.85 0.02 2 79 15 15 SER HB3 H 3.92 0.02 2 80 16 16 THR H H 8.37 0.02 1 81 16 16 THR HA H 4.3 0.02 1 82 16 16 THR HB H 4.19 0.02 1 83 16 16 THR HG2 H 1.21 0.02 1 84 17 17 SET H H 8.6 0.02 1 85 17 17 SET HA H 4.26 0.02 1 86 17 17 SET HB2 H 3.92 0.02 2 87 17 17 SET HB3 H 3.97 0.02 2 stop_ loop_ _Atom_shift_assign_ID_ambiguity 49 '50,53' stop_ save_ ######################## # Coupling constants # ######################## save_coupling_constant_list_1 _Saveframe_category coupling_constants 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 1 NLQ H 1 NLQ HA 7.1 . . 1.5 2 3JHNHA 2 THR H 2 THR HA 7.1 . . 1.5 3 3JHNHA 5 LYS H 5 LYS HA 6.9 . . 1.5 4 3JHNHA 7 SER H 7 SER HA 6.9 . . 1.5 5 3JHNHA 8 ASP H 8 ASP HA 6.5 . . 1.5 6 3JHNHA 10 THR H 10 THR HA 6.9 . . 1.5 7 3JHNHA 11 THR H 11 THR HA 6.5 . . 1.5 8 3JHNHA 13 TYR H 13 TYR HA 6.5 . . 1.5 9 3JHNHA 15 SER H 15 SER HA 6.9 . . 1.5 10 3JHNHA 16 THR H 16 THR HA 8.7 . . 1.5 stop_ save_