data_6941 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; '1H, 13C, and 15N Chemical Shift Assignments for Ac-Dab-Dab-(Ala)7-Orn-Orn-NH2 where Dab-diaminobutyric acid; Orn - ornithine' ; loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Makowska Joanna . . 2 Rodziewicz-Motowidlo Sylwia . . 3 Baginska Katarzyna . . 4 Vila Jorge A. . 5 Liwo Adam . . 6 Chmurzynski Lech K. . 7 Scheraga Harold A. . stop_ _BMRB_accession_number 6941 _BMRB_flat_file_name bmr6941.str _Entry_type new _Submission_date 2004-01-17 _Accession_date 2004-01-17 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 55 "13C chemical shifts" 28 "15N chemical shifts" 12 stop_ save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_title ; Polyproline II conformation is one of many possible local conformational states and is not an overall conformation of unfolded peptides and proteins ; _Citation_status published _Citation_type journal _PubMed_ID 16446433 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Makowska Joanna . . 2 Rodziewicz-Motowidlo Sylwia . . 3 Baginska Katarzyna . . 4 Vila Jorge A. . 5 Liwo Adam . . 6 Chmurzynski Lech K. . 7 Scheraga Harold A. . stop_ _Journal_abbreviation "Proc. Natl. Acad. Sci. U.S.A." _Journal_volume 103 _Journal_issue 6 _Page_first 1744 _Page_last 1749 _Year 2006 save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name XAO _Abbreviation_common XAO loop_ _Mol_system_component_name _Mol_label "subunit 1" $XAO stop_ _System_molecular_weight 985.5 _System_physical_state unfolded _System_oligomer_state monomer _System_paramagnetic no _System_thiol_state "not present" _Details Ac-Dab-Dab-(Ala)7-Orn-Orn-NH2 save_ ######################## # Monomeric polymers # ######################## save_XAO _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common XAO _Name_variant XAO _Abbreviation_common XAO _Molecular_mass 985.5 _Mol_thiol_state "not present" ############################## # Polymer residue sequence # ############################## _Residue_count 11 _Mol_residue_sequence ; XXAAAAAAAXX ; loop_ _Residue_seq_code _Residue_label 1 DAB 2 DAB 3 ALA 4 ALA 5 ALA 6 ALA 7 ALA 8 ALA 9 ALA 10 ORN 11 ORN stop_ save_ ###################### # Polymer residues # ###################### save_DAB _Saveframe_category polymer_residue _Mol_type non-polymer _Name_common "2,4-diaminobutyric acid" _Abbreviation_common "2,4-diaminobutyric acid" _BMRB_code DAB _PDB_code DAB _Standard_residue_derivative ? _Mol_empirical_formula "C4 H8 N2 O1" _Mol_paramagnetic no _Details . loop_ _Atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N ? 0 ? ? CA C ? 0 ? ? C C ? 0 ? ? O O ? 0 ? ? CB C ? 0 ? ? CG C ? 0 ? ? ND N ? 0 ? ? H H ? 0 ? ? HA H ? 0 ? ? HB2 H ? 0 ? ? HB3 H ? 0 ? ? HG2 H ? 0 ? ? HG3 H ? 0 ? ? HD2 H ? 0 ? ? HD3 H ? 0 ? ? N H ? 0 ? ? CA H ? 0 ? ? C H ? 0 ? ? O H ? 0 ? ? CB H ? 0 ? ? CG H ? 0 ? ? ND H ? 0 ? ? H H ? 0 ? ? HA H ? 0 ? ? HB2 H ? 0 ? ? HB3 H ? 0 ? ? HG2 H ? 0 ? ? HG3 H ? 0 ? ? HD2 H ? 0 ? ? HD3 H ? 0 ? ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name SING N CA SING N H SING CA C SING CA CB SING CA HA DOUB C O SING CB CG SING CB HB2 SING CB HB3 SING CG ND SING CG HG2 SING CG HG3 SING ND HD2 SING ND HD3 SING N CA SING N H SING CA C SING CA CB SING CA HA DOUB C O SING CB CG SING CB HB2 SING CB HB3 SING CG ND SING CG HG2 SING CG HG3 SING ND HD2 SING ND HD3 stop_ save_ save_ORN _Saveframe_category polymer_residue _Mol_type non-polymer _Name_common L-ornithine _Abbreviation_common L-ornithine _Name_IUPAC "L-2,5-Diamino valeric acid" _BMRB_code ORN _PDB_code ORN _Standard_residue_derivative ? _Mol_empirical_formula "C5 H10 N2 O1" _Mol_paramagnetic no _Details . loop_ _Atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons N N ? 0 ? ? CA C ? 0 ? ? C C ? 0 ? ? O O ? 0 ? ? CB C ? 0 ? ? CG C ? 0 ? ? CD C ? 0 ? ? NE N ? 0 ? ? H H ? 0 ? ? HA H ? 0 ? ? HB2 H ? 0 ? ? HB3 H ? 0 ? ? HG2 H ? 0 ? ? HG3 H ? 0 ? ? HD2 H ? 0 ? ? HD3 H ? 0 ? ? HNE2 H ? 0 ? ? HNE3 H ? 0 ? ? N H ? 0 ? ? CA H ? 0 ? ? C H ? 0 ? ? O H ? 0 ? ? CB H ? 0 ? ? CG H ? 0 ? ? CD H ? 0 ? ? NE H ? 0 ? ? H H ? 0 ? ? HA H ? 0 ? ? HB2 H ? 0 ? ? HB3 H ? 0 ? ? HG2 H ? 0 ? ? HG3 H ? 0 ? ? HD2 H ? 0 ? ? HD3 H ? 0 ? ? HNE2 H ? 0 ? ? HNE3 H ? 0 ? ? stop_ loop_ _Bond_order _Bond_atom_one_atom_name _Bond_atom_two_atom_name SING N CA SING N H SING CA C SING CA CB SING CA HA DOUB C O SING CB CG SING CB HB2 SING CB HB3 SING CG CD SING CG HG2 SING CG HG3 SING CD NE SING CD HD2 SING CD HD3 SING NE HNE2 SING NE HNE3 SING N CA SING N H SING CA C SING CA CB SING CA HA DOUB C O SING CB CG SING CB HB2 SING CB HB3 SING CG CD SING CG HG2 SING CG HG3 SING CD NE SING CD HD2 SING CD HD3 SING NE HNE2 SING NE HNE3 stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $XAO ? ? ? ? ? ? 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 $XAO "chemical synthesis" ? ? ? ? ? stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details ; The molecule was dissolved in acetate buffer ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $XAO 4 mM ? "sodium acetate buffer" 30 mM ? D2O 10 % ? H2O 90 % ? stop_ save_ ############################ # Computer software used # ############################ save_software_2 _Saveframe_category software _Name XEASY loop_ _Vendor _Address _Electronic_address 1 ? http://spin.niddk.nih.gov/NMRPipe/ 2 ? http://hugin.ethz.ch/wuthrich/software/xeasy/index.html stop_ loop_ _Task "NMR data processing" "peak assignments" stop_ _Details ; F._Delaglio,_S._Grzesiek,_G._W._Vuister,_G._Zhu,_J._Pfeifer_and_A._Bax,_J._Biomol._NMR._6,_277-293_(1995) Bartles_C,_Xia_T,_Billeter_M,_G?nter_P,_W?thrich_K._(1995)_J._Biomol._NMR_5,_1-10. ; save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_500MHz_spectrometer _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model "Varian Unity 500 Plus" _Field_strength 500 save_ ############################# # NMR applied experiments # ############################# save_1D_NMR _Saveframe_category NMR_applied_experiment _Experiment_name "1D NMR" _Sample_label $sample_1 save_ save_1H1H_TOCSY _Saveframe_category NMR_applied_experiment _Experiment_name "1H1H TOCSY" _Sample_label $sample_1 save_ save_1H1H_NOESY _Saveframe_category NMR_applied_experiment _Experiment_name "1H1H NOESY" _Sample_label $sample_1 save_ save_1H1H_ROESY _Saveframe_category NMR_applied_experiment _Experiment_name "1H1H ROESY" _Sample_label $sample_1 save_ save_1H13C_HSQC _Saveframe_category NMR_applied_experiment _Experiment_name "1H13C HSQC" _Sample_label $sample_1 save_ save_1H15N_HSQC _Saveframe_category NMR_applied_experiment _Experiment_name "1H15N HSQC" _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_conditions_1 _Saveframe_category sample_conditions _Details ; The XAO peptide was dissolved in 30 mM sodium acetate buffer (pH 4.5 in 10 % D2O). The peptide concentration was 4 mM. All 2D NMR spectra were recorded at 5oC except for the temperature coefficients of the chemical shifts, which were measured throughout the temperature range 5-44 oC. ; loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 4.5 0.01 pH temperature 5 0.01 C stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chemical_shift_referencing _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 0.0 internal direct ? ? ? 1.0 DSS C 13 "methyl protons" ppm 0.0 . indirect ? ? ? 0.251449530 DSS N 15 "methyl protons" ppm 0.0 . indirect ? ? ? 0.101329118 stop_ save_ ################################### # Assigned chemical shift lists # ################################### ################################################################### # Chemical Shift Ambiguity Index Value Definitions # # # # Index Value Definition # # # # 1 Unique (geminal atoms and geminal methyl # # groups with identical chemical shifts # # are assumed to be assigned to # # stereospecific atoms) # # 2 Ambiguity of geminal atoms or geminal methyl # # proton groups # # 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) # # 9 Ambiguous, specific ambiguity not defined # # # ################################################################### save_chem_shift_list_1 _Saveframe_category assigned_chemical_shifts loop_ _Software_label $software_2 stop_ loop_ _Experiment_label $1D_NMR $1H1H_TOCSY $1H1H_NOESY $1H1H_ROESY $1H13C_HSQC $1H15N_HSQC stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $conditions_1 _Chem_shift_reference_set_label $chemical_shift_referencing _Mol_system_component_name "subunit 1" loop_ _Atom_shift_assign_ID _Residue_seq_code _Residue_label _Atom_name _Atom_type _Chem_shift_value _Chem_shift_value_error _Chem_shift_ambiguity_code 1 1 DAB H1 H 2.04 0.012 1 2 1 DAB HA H 4.36 0.012 1 3 1 DAB HB2 H 2.14 0.012 1 4 1 DAB HB3 H 2.05 0.012 1 5 1 DAB HG2 H 3.08 0.012 2 6 1 DAB HG3 H 3.08 0.012 2 7 1 DAB HZ H 7.81 0.012 5 8 1 DAB CA C 54.31 0.003 1 9 1 DAB CB C 31.50 0.003 1 10 1 DAB CG C 39.10 0.003 1 11 1 DAB N N 125 0.003 9 12 1 DAB H H 8.63 0.012 1 13 2 DAB H H 8.85 0.012 1 14 2 DAB HA H 4.42 0.012 1 15 2 DAB HB2 H 2.17 0.012 1 16 2 DAB HB3 H 2.08 0.012 1 17 2 DAB HG2 H 3.08 0.012 2 18 2 DAB HG3 H 3.08 0.012 2 19 2 DAB HZ H 7.81 0.012 5 20 2 DAB CA C 53.98 0.003 1 21 2 DAB CB C 31.58 0.003 1 22 2 DAB CG C 39.10 0.003 1 23 2 DAB N N 121.04 0.003 1 24 3 ALA H H 8.64 0.012 1 25 3 ALA HA H 4.25 0.012 1 26 3 ALA HB H 1.39 0.012 1 27 3 ALA CA C 52.54 0.003 1 28 3 ALA CB C 19.14 0.003 1 29 3 ALA N N 124.13 0.003 1 30 4 ALA H H 8.55 0.012 1 31 4 ALA HA H 4.24 0.012 1 32 4 ALA HB H 1.39 0.012 1 33 4 ALA CA C 52.54 0.003 1 34 4 ALA CB C 19.14 0.003 1 35 4 ALA N N 124.56 0.003 1 36 5 ALA H H 8.47 0.012 1 37 5 ALA HA H 4.23 0.012 1 38 5 ALA HB H 1.39 0.012 1 39 5 ALA CA C 52.54 0.003 1 40 5 ALA CB C 19.14 0.003 1 41 5 ALA N N 124.44 0.003 1 42 6 ALA H H 8.44 0.012 1 43 6 ALA HA H 4.23 0.012 1 44 6 ALA HB H 1.39 0.012 1 45 6 ALA CA C 52.54 0.003 1 46 6 ALA CB C 19.14 0.003 1 47 6 ALA N N 124.17 0.003 1 48 7 ALA H H 8.40 0.012 1 49 7 ALA HA H 4.23 0.012 . 50 7 ALA HB H 1.39 0.012 1 51 7 ALA CA C 52.54 0.003 1 52 7 ALA CB C 19.14 0.003 1 53 7 ALA N N 124.04 0.003 1 54 8 ALA H H 8.34 0.012 1 55 8 ALA HA H 4.24 0.012 1 56 8 ALA HB H 1.39 0.012 1 57 8 ALA CA C 52.54 0.003 1 58 8 ALA CB C 19.14 0.003 1 59 8 ALA N N 123.84 0.003 1 60 9 ALA H H 8.36 0.012 1 61 9 ALA HA H 4.24 0.012 1 62 9 ALA HB H 1.39 0.012 1 63 9 ALA CA C 52.54 0.003 1 64 9 ALA CB C 19.14 0.003 1 65 9 ALA N N 124.01 0.003 1 66 10 ORN H H 8.51 0.012 1 67 10 ORN HA H 4.31 0.012 1 68 10 ORN HB2 H 1.87 0.012 1 69 10 ORN HB3 H 1.79 0.012 1 70 10 ORN HG2 H 1.78 0.012 2 71 10 ORN HG3 H 1.78 0.012 2 72 10 ORN HD2 H 3.02 0.012 2 73 10 ORN HD3 H 3.02 0.012 2 74 10 ORN HZ H 7.69 0.012 5 75 10 ORN CA C 55.89 0.003 1 76 10 ORN CB C 30.68 0.003 1 77 10 ORN CG C 26.13 0.003 1 78 10 ORN CD C 41.79 0.003 1 79 10 ORN N N 121.14 0.003 1 80 11 ORN H H 8.63 0.012 1 81 11 ORN HA H 4.30 0.012 1 82 11 ORN HB2 H 1.88 0.012 1 83 11 ORN HB3 H 1.79 0.012 1 84 11 ORN HG2 H 1.73 0.012 2 85 11 ORN HG3 H 1.72 0.012 2 86 11 ORN HD2 H 3.02 0.012 2 87 11 ORN HD3 H 3.02 0.012 2 88 11 ORN HZ H 7.69 0.012 5 89 11 ORN H1 H 7.28 0.012 1 90 11 ORN CA C 55.89 0.003 1 91 11 ORN CB C 30.68 0.003 1 92 11 ORN CG C 26.13 0.003 1 93 11 ORN CD C 41.79 0.003 1 94 11 ORN N N 125.0 0.003 9 95 11 ORN NH2 N 109.45 0.003 1 stop_ loop_ _Atom_shift_assign_ID_ambiguity 7 19 '74,88' stop_ save_