data_15099 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Solution structure of CM15 in DPC micelles ; _BMRB_accession_number 15099 _BMRB_flat_file_name bmr15099.str _Entry_type original _Submission_date 2007-01-10 _Accession_date 2007-01-10 _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 Respondek Michal . . 2 Madl Tobias . . 3 Goebl Christoph . . 4 Golser Regina . . 5 Zangger Klaus . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 66 "13C chemical shifts" 26 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2008-07-01 update BMRB 'complete entry citation' 2007-09-12 original author 'original release' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Mapping the orientation of helices in micelle-bound peptides by paramagnetic relaxation waves' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 17397158 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Respondek Michal . . 2 Madl Tobias . . 3 Goebl Christoph . . 4 Golser Regina . . 5 Zangger Klaus . . stop_ _Journal_abbreviation 'J. Am. Chem. Soc.' _Journal_volume 129 _Journal_issue 16 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 5228 _Page_last 5234 _Year 2007 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'CM15 in DPC micelles' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label CM15 $CM15 stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic ? _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_CM15 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common CM15 _Molecular_mass 1776.343 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 15 _Mol_residue_sequence KWKLFKKIGAVLKVL loop_ _Residue_seq_code _Residue_label 1 LYS 2 TRP 3 LYS 4 LEU 5 PHE 6 LYS 7 LYS 8 ILE 9 GLY 10 ALA 11 VAL 12 LEU 13 LYS 14 VAL 15 LEU stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $CM15 . . . . Synthetic Synthetic 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 $CM15 'chemical synthesis' . not applicable . . 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 _Isotopic_labeling $CM15 1.7 mM 'natural abundance' DPC 100 mM [U-2H] KPi 50 mM 'natural abundance' 'Sodium azide' 0.02 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CNS _Saveframe_category software _Name CNS _Version 1.1 loop_ _Vendor _Address _Electronic_address 'Brunger, Adams, Clore, Gros, Nilges and Read' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 500 _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_1 save_ save_2D_1H-1H_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_1 save_ save_2D_1H-13C_HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _Sample_label $sample_1 save_ save_HNCACO_4 _Saveframe_category NMR_applied_experiment _Experiment_name HNCACO _Sample_label $sample_1 save_ save_2D_1H-15N_HSQC_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_3D_CCH-TOCSY_6 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CCH-TOCSY' _Sample_label $sample_1 save_ save_3D_HNCA_7 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCA' _Sample_label $sample_1 save_ save_3D_HBHACANH_8 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HBHACANH' _Sample_label $sample_1 save_ save_3D_1H-13C_NOESY_9 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-13C NOESY' _Sample_label $sample_1 save_ save_3D_HCCH-TOCSY_10 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-TOCSY' _Sample_label $sample_1 save_ save_3D_HNCOCA_11 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCOCA' _Sample_label $sample_1 save_ save_3D_HCCH-COSY_arom_12 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-COSY arom' _Sample_label $sample_1 save_ save_3D_1H-13C_NOESY-HSQC_13 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-13C NOESY-HSQC' _Sample_label $sample_1 save_ save_3D_CCCONH_14 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CCCONH' _Sample_label $sample_1 save_ save_3D_HNCOCACB_15 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCOCACB' _Sample_label $sample_1 save_ save_3D_HCCH-COSY_RD1_16 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-COSY RD1' _Sample_label $sample_1 save_ save_3D_HNCO_17 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCO' _Sample_label $sample_1 save_ save_3D_HNHA_18 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNHA' _Sample_label $sample_1 save_ save_3D_HCCH-COSY_19 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-COSY' _Sample_label $sample_1 save_ save_3D_HBHACACONH_20 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HBHACACONH' _Sample_label $sample_1 save_ save_3D_HNCACB_21 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HNCACB' _Sample_label $sample_1 save_ save_3D_CBCACONH_22 _Saveframe_category NMR_applied_experiment _Experiment_name '3D CBCACONH' _Sample_label $sample_1 save_ save_3D_1H-15N_NOESY_23 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-15N NOESY' _Sample_label $sample_1 save_ save_3D_HCCCONH_TOCSY_24 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCCONH TOCSY' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details ; 100 mM deuterated DPC (dodecylphosphocholine) ; loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0.15 . M pH 5.0 . pH pressure 1 . atm temperature 305 . 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 DSS C 13 'methyl carbons' ppm 0.0 external direct . . . 1.0 $entry_citation $entry_citation DSS H 1 'methyl protons' ppm 0.0 external direct . . . 1.0 $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 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H TOCSY' '2D 1H-13C HSQC' 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 CM15 _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 LYS H H 8.712 . 1 2 1 1 LYS HA H 3.870 . 1 3 1 1 LYS HB2 H 1.584 . 2 4 1 1 LYS HG2 H 1.207 . 2 5 1 1 LYS HD2 H 1.557 . 2 6 1 1 LYS HE2 H 2.818 . 2 7 1 1 LYS CA C 58.00 . 1 8 1 1 LYS CB C 28.10 . 1 9 2 2 TRP H H 8.394 . 1 10 2 2 TRP HA H 4.760 . 1 11 2 2 TRP HB2 H 3.312 . 2 12 2 2 TRP HD1 H 7.341 . 1 13 2 2 TRP HE1 H 10.653 . 1 14 2 2 TRP HE3 H 7.497 . 1 15 2 2 TRP HZ2 H 7.509 . 1 16 2 2 TRP HZ3 H 6.837 . 1 17 2 2 TRP HH2 H 7.074 . 1 18 2 2 TRP CB C 27.80 . 1 19 3 3 LYS H H 7.804 . 1 20 3 3 LYS HA H 3.905 . 1 21 3 3 LYS HB2 H 1.995 . 2 22 3 3 LYS CA C 58.00 . 1 23 3 3 LYS CB C 31.10 . 1 24 4 4 LEU H H 7.864 . 1 25 4 4 LEU HA H 4.049 . 1 26 4 4 LEU HB2 H 1.670 . 2 27 4 4 LEU HG H 1.651 . 1 28 4 4 LEU HD1 H 0.834 . 2 29 4 4 LEU CA C 56.80 . 1 30 4 4 LEU CB C 40.40 . 1 31 5 5 PHE H H 8.154 . 1 32 5 5 PHE HA H 4.184 . 1 33 5 5 PHE HB2 H 3.155 . 2 34 5 5 PHE HD1 H 7.069 . 1 35 5 5 PHE CA C 60.50 . 1 36 5 5 PHE CB C 37.10 . 1 37 6 6 LYS H H 8.033 . 1 38 6 6 LYS HA H 3.931 . 1 39 6 6 LYS HB2 H 1.846 . 2 40 6 6 LYS HG2 H 1.389 . 2 41 6 6 LYS CA C 58.20 . 1 42 6 6 LYS CB C 31.10 . 1 43 7 7 LYS H H 7.745 . 1 44 7 7 LYS HA H 4.170 . 1 45 7 7 LYS HB2 H 1.899 . 2 46 7 7 LYS HG2 H 1.658 . 2 47 7 7 LYS HE2 H 2.912 . 2 48 7 7 LYS CA C 57.50 . 1 49 8 8 ILE H H 8.069 . 1 50 8 8 ILE HA H 3.672 . 1 51 8 8 ILE HB H 1.833 . 1 52 8 8 ILE HG12 H 0.845 . 2 53 8 8 ILE HD1 H 0.776 . 1 54 8 8 ILE CA C 63.70 . 1 55 8 8 ILE CB C 36.80 . 1 56 9 9 GLY H H 8.409 . 1 57 9 9 GLY HA2 H 3.670 . 2 58 9 9 GLY CA C 46.50 . 1 59 10 10 ALA H H 7.769 . 1 60 10 10 ALA HA H 4.105 . 1 61 10 10 ALA HB H 1.518 . 1 62 10 10 ALA CA C 53.80 . 1 63 10 10 ALA CB C 17.40 . 1 64 11 11 VAL H H 7.681 . 1 65 11 11 VAL HA H 3.755 . 1 66 11 11 VAL HB H 2.260 . 1 67 11 11 VAL HG1 H 0.994 . 2 68 11 11 VAL CA C 64.40 . 1 69 11 11 VAL CB C 30.80 . 1 70 12 12 LEU H H 8.055 . 1 71 12 12 LEU HA H 3.966 . 1 72 12 12 LEU HB2 H 1.980 . 2 73 12 12 LEU HD1 H 0.813 . 2 74 12 12 LEU CA C 56.50 . 1 75 13 13 LYS H H 7.753 . 1 76 13 13 LYS HA H 3.961 . 1 77 13 13 LYS HB2 H 1.808 . 2 78 13 13 LYS HE2 H 2.919 . 2 79 13 13 LYS CA C 57.80 . 1 80 13 13 LYS CB C 31.10 . 1 81 14 14 VAL H H 7.337 . 1 82 14 14 VAL HA H 3.943 . 1 83 14 14 VAL HB H 2.258 . 1 84 14 14 VAL HG1 H 1.002 . 2 85 14 14 VAL CA C 63.00 . 1 86 14 14 VAL CB C 30.80 . 1 87 15 15 LEU H H 7.653 . 1 88 15 15 LEU HA H 4.059 . 1 89 15 15 LEU HB2 H 1.800 . 2 90 15 15 LEU HD1 H 0.829 . 2 91 15 15 LEU CA C 55.00 . 1 92 15 15 LEU CB C 40.40 . 1 stop_ save_