data_15241 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; 1H Chemical shift assignments for [Nle15] gastrin-17 in the presence of DPC micelles. ; _BMRB_accession_number 15241 _BMRB_flat_file_name bmr15241.str _Entry_type original _Submission_date 2007-05-08 _Accession_date 2007-05-08 _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 Stone Shane R. . 2 Mierke Dale F. . 3 Jackson Graham E. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 171 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2007-10-29 original author . stop_ _Original_release_date 2007-10-29 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Evidence for a C-terminal Structural Motif in Gastrin and its Bioactive Fragments in Membrane Mimetic Media.' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 17698249 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Stone Shane R. . 2 Mierke Dale F. . 3 Jackson Graham E. . stop_ _Journal_abbreviation Peptides _Journal_volume 28 _Journal_issue 8 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 1561 _Page_last 1571 _Year 2007 _Details . loop_ _Keyword cholecystokinin DPC gastrin 'membrane mimetic media' micelles stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name '[Nle15] gastrin-17' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label '[Nle15] gastrin-17, major' $Nle15_Gastrin-17 '[Nle15] gastrin-17, minor' $Nle15_Gastrin-17 stop_ _System_molecular_weight 2080.3 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . loop_ _Biological_function 'gastric acid secretion' stop_ _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_Nle15_Gastrin-17 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common Nle15_Gastrin-17 _Molecular_mass . _Mol_thiol_state 'not present' _Details 'C-terminal is amidated' ############################## # Polymer residue sequence # ############################## _Residue_count 18 _Mol_residue_sequence XGPWLEEEEEAYGWXDFX loop_ _Residue_seq_code _Residue_label 1 PCA 2 GLY 3 PRO 4 TRP 5 LEU 6 GLU 7 GLU 8 GLU 9 GLU 10 GLU 11 ALA 12 TYR 13 GLY 14 TRP 15 NLE 16 ASP 17 PHE 18 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_PCA _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common 'PYROGLUTAMIC ACID' _BMRB_code . _PDB_code PCA _Standard_residue_derivative . _Molecular_mass 129.114 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Fri Oct 14 10:26:05 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 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD CD C . 0 . ? OE OE O . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 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 CD ? ? SING N H ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD ? ? SING CG HG2 ? ? SING CG HG3 ? ? DOUB CD OE ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? stop_ save_ save_chem_comp_NLE _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common NORLEUCINE _BMRB_code . _PDB_code NLE _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 Oct 14 10:27:52 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 . ? OXT OXT O . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD CD C . 0 . ? CE CE C . 0 . ? H H H . 0 . ? HN2 HN2 H . 0 . ? HA HA H . 0 . ? HXT HXT H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HG2 HG2 H . 0 . ? HG3 HG3 H . 0 . ? HD2 HD2 H . 0 . ? HD3 HD3 H . 0 . ? HE1 HE1 H . 0 . ? HE2 HE2 H . 0 . ? HE3 HE3 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 HN2 ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CG CD ? ? SING CG HG2 ? ? SING CG HG3 ? ? SING CD CE ? ? SING CD HD2 ? ? SING CD HD3 ? ? SING CE HE1 ? ? SING CE HE2 ? ? SING CE HE3 ? ? stop_ save_ save_chem_comp_NH2 _Saveframe_category polymer_residue _Mol_type non-polymer _Name_common 'AMINO GROUP' _BMRB_code . _PDB_code NH2 _Standard_residue_derivative . _Molecular_mass 16.023 _Mol_paramagnetic . _Details ; Information obtained from PDB's Chemical Component Dictionary at http://wwpdb-remediation.rutgers.edu/downloads.html Downloaded on Fri Oct 14 10:30:40 2011 ; loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N N . 0 . ? HN1 HN1 H . 0 . ? HN2 HN2 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 HN1 ? ? SING N HN2 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $Nle15_Gastrin-17 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 $Nle15_Gastrin-17 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample _Saveframe_category sample _Sample_type micelle _Details 'Sample volume was 0.6 ml containing 50mM phosphate buffer, 150 mM DPC, ca 1.5 mM [Nle15] gastrin-17 and 90:10 H2O:D2O.' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling TSP 0.1 mM 'natural abundance' $assembly 1.5 mM 'natural abundance' 'phosphate buffer' 50 mM 'natural abundance' DPC 150 mM '[U-99% 2H]' H2O 90 % 'natural abundance' D2O 10 % '[U-99% 2H]' stop_ save_ ############################ # Computer software used # ############################ save_NMRPipe _Saveframe_category software _Name NMRPipe _Version . loop_ _Vendor _Address _Electronic_address 'Delaglio, Grzesiek, Vuister, Zhu, Pfeifer and Bax' . . stop_ loop_ _Task processing stop_ _Details . save_ save_SPARKY _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_TOCSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample save_ save_2D_1H-1H_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details 'Sample volume was 0.6 ml containing 50mM phosphate buffer, 150 mM DPC, ca 1.5 mM [Nle15] gastrin-17 and 90:10 H2O:D2O.' loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 50 . mM pH 5.2 . pH pressure 1 . atm temperature 308 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_reference_1 _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 _Indirect_shift_ratio_citation_label _Correction_value_citation_label TSP H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 $entry_citation $entry_citation 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_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $NMRPipe $SPARKY stop_ loop_ _Experiment_label '2D 1H-1H TOCSY' '2D 1H-1H NOESY' stop_ loop_ _Sample_label $sample stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name '[Nle15] gastrin-17, major' _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 PCA H H 8.39 0.01 1 2 1 1 PCA HA H 4.36 0.01 1 3 1 1 PCA HB2 H 1.95 0.01 1 4 1 1 PCA HB3 H 2.05 0.01 1 5 1 1 PCA HG2 H 2.40 0.01 2 6 1 1 PCA HG3 H 2.40 0.01 2 7 2 2 GLY H H 8.35 0.01 1 8 2 2 GLY HA2 H 3.98 0.01 1 9 2 2 GLY HA3 H 4.09 0.01 1 10 3 3 PRO HA H 4.43 0.01 1 11 3 3 PRO HB2 H 2.05 0.01 1 12 3 3 PRO HB3 H 2.22 0.01 1 13 3 3 PRO HG2 H 1.83 0.01 1 14 3 3 PRO HG3 H 1.92 0.01 1 15 3 3 PRO HD2 H 3.68 0.01 2 16 3 3 PRO HD3 H 3.68 0.01 2 17 4 4 TRP H H 8.25 0.01 1 18 4 4 TRP HA H 4.57 0.01 1 19 4 4 TRP HB2 H 3.29 0.01 2 20 4 4 TRP HB3 H 3.29 0.01 2 21 4 4 TRP HD1 H 7.31 0.01 1 22 4 4 TRP HE1 H 10.52 0.01 1 23 4 4 TRP HE3 H 7.54 0.01 1 24 5 5 LEU H H 7.92 0.01 1 25 5 5 LEU HA H 4.16 0.01 1 26 5 5 LEU HB2 H 1.61 0.01 1 27 5 5 LEU HB3 H 1.56 0.01 1 28 5 5 LEU HG H 1.48 0.01 1 29 5 5 LEU HD1 H 0.85 0.01 1 30 5 5 LEU HD2 H 0.81 0.01 1 31 6 6 GLU H H 8.15 0.01 1 32 6 6 GLU HA H 4.10 0.01 1 33 6 6 GLU HB2 H 2.05 0.01 1 34 6 6 GLU HB3 H 1.97 0.01 1 35 6 6 GLU HG2 H 2.27 0.01 2 36 6 6 GLU HG3 H 2.27 0.01 2 37 7 7 GLU H H 8.24 0.01 1 38 7 7 GLU HA H 4.20 0.01 1 39 7 7 GLU HB2 H 2.05 0.01 2 40 7 7 GLU HB3 H 2.05 0.01 2 41 7 7 GLU HG2 H 2.32 0.01 2 42 7 7 GLU HG3 H 2.32 0.01 2 43 8 8 GLU H H 8.21 0.01 1 44 8 8 GLU HA H 4.16 0.01 1 45 8 8 GLU HB2 H 2.06 0.01 1 46 8 8 GLU HB3 H 2.01 0.01 1 47 8 8 GLU HG2 H 2.25 0.01 2 48 8 8 GLU HG3 H 2.25 0.01 2 49 9 9 GLU H H 8.28 0.01 1 50 9 9 GLU HA H 4.02 0.01 1 51 9 9 GLU HB2 H 2.05 0.01 2 52 9 9 GLU HB3 H 2.05 0.01 2 53 9 9 GLU HG2 H 2.39 0.01 1 54 9 9 GLU HG3 H 2.26 0.01 1 55 10 10 GLU H H 8.11 0.01 1 56 10 10 GLU HA H 4.13 0.01 1 57 10 10 GLU HB2 H 2.03 0.01 2 58 10 10 GLU HB3 H 2.03 0.01 2 59 10 10 GLU HG2 H 2.34 0.01 1 60 10 10 GLU HG3 H 2.27 0.01 1 61 11 11 ALA H H 7.98 0.01 1 62 11 11 ALA HA H 3.98 0.01 1 63 11 11 ALA HB H 1.24 0.01 1 64 12 12 TYR H H 7.95 0.01 1 65 12 12 TYR HA H 4.30 0.01 1 66 12 12 TYR HB2 H 2.91 0.01 1 67 12 12 TYR HB3 H 2.82 0.01 1 68 12 12 TYR HD1 H 7.02 0.01 3 69 12 12 TYR HD2 H 7.02 0.01 3 70 12 12 TYR HE1 H 6.78 0.01 3 71 12 12 TYR HE2 H 6.78 0.01 3 72 13 13 GLY H H 8.05 0.01 1 73 13 13 GLY HA2 H 4.03 0.01 1 74 13 13 GLY HA3 H 3.89 0.01 1 75 14 14 TRP H H 7.66 0.01 1 76 14 14 TRP HA H 4.47 0.01 1 77 14 14 TRP HB2 H 3.39 0.01 1 78 14 14 TRP HB3 H 3.26 0.01 1 79 14 14 TRP HD1 H 7.36 0.01 1 80 14 14 TRP HE1 H 10.44 0.01 1 81 14 14 TRP HE3 H 7.49 0.01 1 82 15 15 NLE H H 7.35 0.01 1 83 15 15 NLE HA H 3.91 0.01 1 84 15 15 NLE HB2 H 1.50 0.01 1 85 15 15 NLE HB3 H 1.39 0.01 1 86 15 15 NLE HG2 H 1.24 0.01 1 87 15 15 NLE HG3 H 1.15 0.01 1 88 15 15 NLE HD2 H 0.93 0.01 1 89 15 15 NLE HD3 H 0.87 0.01 1 90 16 16 ASP H H 7.59 0.01 1 91 16 16 ASP HA H 4.52 0.01 1 92 16 16 ASP HB2 H 2.72 0.01 1 93 16 16 ASP HB3 H 2.45 0.01 1 94 17 17 PHE H H 8.01 0.01 1 95 17 17 PHE HA H 4.48 0.01 1 96 17 17 PHE HB2 H 3.21 0.01 1 97 17 17 PHE HB3 H 2.97 0.01 1 98 17 17 PHE HD1 H 7.26 0.01 3 99 17 17 PHE HD2 H 7.26 0.01 3 100 17 17 PHE HE1 H 7.14 0.01 3 101 17 17 PHE HE2 H 7.14 0.01 3 102 18 18 NH2 HN1 H 7.60 0.01 1 103 18 18 NH2 HN2 H 6.97 0.01 1 stop_ save_ save_assigned_chem_shift_list_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Software_label $NMRPipe $SPARKY stop_ loop_ _Experiment_label '2D 1H-1H TOCSY' '2D 1H-1H NOESY' stop_ loop_ _Sample_label $sample stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name '[Nle15] gastrin-17, minor' _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 2 GLY H H 8.21 0.01 1 2 2 2 GLY HA2 H 3.52 0.01 1 3 2 2 GLY HA3 H 2.95 0.01 1 4 3 3 PRO HA H 4.44 0.01 1 5 3 3 PRO HB2 H 2.28 0.01 1 6 3 3 PRO HB3 H 2.03 0.01 1 7 3 3 PRO HG2 H 1.80 0.01 1 8 3 3 PRO HG3 H 1.56 0.01 1 9 3 3 PRO HD2 H 3.42 0.01 2 10 3 3 PRO HD3 H 3.42 0.01 2 11 4 4 TRP H H 8.59 0.01 1 12 4 4 TRP HA H 4.76 0.01 1 13 4 4 TRP HB2 H 3.34 0.01 2 14 4 4 TRP HB3 H 3.19 0.01 2 15 4 4 TRP HD1 H 7.28 0.01 1 16 4 4 TRP HE1 H 10.34 0.01 1 17 4 4 TRP HE3 H 7.62 0.01 1 18 5 5 LEU H H 8.23 0.01 1 19 5 5 LEU HA H 4.36 0.01 1 20 5 5 LEU HB2 H 1.61 0.01 1 21 5 5 LEU HB3 H 1.56 0.01 1 22 5 5 LEU HG H 1.48 0.01 1 23 5 5 LEU HD1 H 0.84 0.01 2 24 5 5 LEU HD2 H 0.84 0.01 2 25 6 6 GLU H H 8.43 0.01 1 26 6 6 GLU HA H 4.20 0.01 1 27 6 6 GLU HB2 H 2.05 0.01 1 28 6 6 GLU HB3 H 1.95 0.01 1 29 6 6 GLU HG2 H 2.29 0.01 2 30 6 6 GLU HG3 H 2.29 0.01 2 31 11 11 ALA H H 8.05 0.01 1 32 11 11 ALA HA H 4.03 0.01 1 33 11 11 ALA HB H 1.23 0.01 1 34 12 12 TYR H H 8.01 0.01 1 35 12 12 TYR HA H 4.30 0.01 1 36 12 12 TYR HB2 H 2.90 0.01 1 37 12 12 TYR HB3 H 2.83 0.01 1 38 13 13 GLY H H 8.15 0.01 1 39 13 13 GLY HA2 H 3.90 0.01 1 40 13 13 GLY HA3 H 3.90 0.01 1 41 14 14 TRP H H 7.69 0.01 1 42 14 14 TRP HA H 4.47 0.01 1 43 14 14 TRP HB2 H 3.39 0.01 1 44 14 14 TRP HB3 H 3.26 0.01 1 45 14 14 TRP HD1 H 7.37 0.01 1 46 14 14 TRP HE1 H 10.48 0.01 1 47 15 15 NLE H H 7.35 0.01 1 48 15 15 NLE HA H 3.91 0.01 1 49 15 15 NLE HB2 H 1.50 0.01 1 50 15 15 NLE HB3 H 1.39 0.01 1 51 15 15 NLE HG2 H 1.24 0.01 1 52 15 15 NLE HG3 H 1.15 0.01 1 53 15 15 NLE HD2 H 0.93 0.01 1 54 15 15 NLE HD3 H 0.87 0.01 1 55 16 16 ASP H H 7.59 0.01 1 56 16 16 ASP HA H 4.52 0.01 1 57 16 16 ASP HB2 H 2.72 0.01 1 58 16 16 ASP HB3 H 2.45 0.01 1 59 17 17 PHE H H 8.01 0.01 1 60 17 17 PHE HA H 4.48 0.01 1 61 17 17 PHE HB2 H 3.21 0.01 1 62 17 17 PHE HB3 H 2.97 0.01 1 63 17 17 PHE HD1 H 7.26 0.01 3 64 17 17 PHE HD2 H 7.26 0.01 3 65 17 17 PHE HE1 H 7.14 0.01 3 66 17 17 PHE HE2 H 7.14 0.01 3 67 18 18 NH2 HN1 H 7.60 0.01 1 68 18 18 NH2 HN2 H 6.97 0.01 1 stop_ save_