data_34060 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR solution structure of Harzianin HK-VI in DPC micelles ; _BMRB_accession_number 34060 _BMRB_flat_file_name bmr34060.str _Entry_type original _Submission_date 2016-11-02 _Accession_date 2016-11-02 _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 Kara S. . . 2 Zamora-Carreras H. . . 3 Afonin S. . . 4 Grage S. L. . 5 Ulrich A. S. . 6 Jimenez M. A. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 85 "13C chemical shifts" 41 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2018-02-23 original BMRB . stop_ _Original_release_date 2016-12-16 save_ ############################# # Citation for this entry # ############################# save_citation_2 _Saveframe_category entry_citation _Citation_full . _Citation_title ; 11-mer peptaibol Harzianin VI: conformational and biological analysis ; _Citation_status 'in preparation' _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID ? loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Kara S. . . 2 Afonin S. . . 3 Zamora-Carreras H. . . 4 Bordessa A. . . 5 Doan V. . . 6 Takeshita N. . . 7 Grage S. L. . 8 Chaume G. . . 9 Jimenez M. A. . 10 Fischer R. . . 11 Bruix M. . . 12 Brigaud T. . . 13 Ulrich A. S. . 14 Rebuffat S. . . 15 Hlimi S. . . 16 Prigent Y. . . 17 Goulard C. . . 18 Bodo B. . . stop_ _Journal_abbreviation . _Journal_volume . _Journal_issue . _Journal_CSD 0353 _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first . _Page_last . _Year . _Details . save_ ####################################### # Cited references within the entry # ####################################### save_citation_1 _Saveframe_category citation _Citation_full . _Citation_title ; Isolation and structural elucidation of the 11-residue peptaibol antibiotic, harzianin HK VI. ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID ? loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Rebuffat Sylvie . . stop_ _Journal_abbreviation 'J. Chem. Soc., Perkin Trans.1' _Journal_name_full . _Journal_volume . _Journal_issue . _Journal_CSD . _Book_title . _Book_chapter_title . _Book_volume . _Book_series . _Book_publisher . _Book_publisher_city . _Book_ISBN . _Conference_title . _Conference_site . _Conference_state_province . _Conference_country . _Conference_start_date . _Conference_end_date . _Conference_abstract_number . _Thesis_institution . _Thesis_institution_city . _Thesis_institution_country . _Page_first 2021 _Page_last 2027 _Year 1996 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name ACE-AIB-ASN-ILE-ILE-AIB-PRO-LEU-LEU-AIB-PRO-LOH _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label entity_1 $entity_1 stop_ _System_molecular_weight . _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_entity_1 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common entity_1 _Molecular_mass 1159.505 _Mol_thiol_state 'not present' _Details http://bioinfo.lifl.fr/norine/result.jsp?ID=NOR00999 ############################## # Polymer residue sequence # ############################## _Residue_count 12 _Mol_residue_sequence ; XXNIIXPLLXPX ; loop_ _Residue_seq_code _Residue_label 1 ACE 2 AIB 3 ASN 4 ILE 5 ILE 6 AIB 7 PRO 8 LEU 9 LEU 10 AIB 11 PRO 12 DCL stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_ACE _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common 'ACETYL GROUP' _BMRB_code ACE _PDB_code ACE _Standard_residue_derivative . _Molecular_mass 44.053 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C C C . 0 . ? O O O . 0 . ? CH3 CH3 C . 0 . ? H H H . 0 . ? H1 H1 H . 0 . ? H2 H2 H . 0 . ? H3 H3 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 DOUB C O ? ? SING C CH3 ? ? SING C H ? ? SING CH3 H1 ? ? SING CH3 H2 ? ? SING CH3 H3 ? ? stop_ save_ save_chem_comp_AIB _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common 'ALPHA-AMINOISOBUTYRIC ACID' _BMRB_code AIB _PDB_code AIB _Standard_residue_derivative . _Molecular_mass 103.120 _Mol_paramagnetic . _Details . 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 . ? CB1 CB1 C . 0 . ? CB2 CB2 C . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HO2 HO2 H . 0 . ? HB11 HB11 H . 0 . ? HB12 HB12 H . 0 . ? HB13 HB13 H . 0 . ? HB21 HB21 H . 0 . ? HB22 HB22 H . 0 . ? HB23 HB23 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 H2 ? ? SING CA C ? ? SING CA CB1 ? ? SING CA CB2 ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HO2 ? ? SING CB1 HB11 ? ? SING CB1 HB12 ? ? SING CB1 HB13 ? ? SING CB2 HB21 ? ? SING CB2 HB22 ? ? SING CB2 HB23 ? ? stop_ save_ save_chem_comp_DCL _Saveframe_category polymer_residue _Mol_type PEPTIDE-LIKE _Name_common 2-AMINO-4-METHYL-PENTAN-1-OL _BMRB_code DCL _PDB_code DCL _Standard_residue_derivative . _Molecular_mass 117.189 _Mol_paramagnetic . _Details . 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 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD1 CD1 C . 0 . ? CD2 CD2 C . 0 . ? OXT OXT O . 0 . ? HN1 HN1 H . 0 . ? HN2 HN2 H . 0 . ? HA HA H . 0 . ? HC1 HC1 H . 0 . ? HC2 HC2 H . 0 . ? HB1 HB1 H . 0 . ? HB2 HB2 H . 0 . ? HG HG H . 0 . ? HD11 HD11 H . 0 . ? HD12 HD12 H . 0 . ? HD13 HD13 H . 0 . ? HD21 HD21 H . 0 . ? HD22 HD22 H . 0 . ? HD23 HD23 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 HN1 ? ? SING N HN2 ? ? SING CA C ? ? SING CA CB ? ? SING CA HA ? ? SING C OXT ? ? SING C HC1 ? ? SING C HC2 ? ? SING CB CG ? ? SING CB HB1 ? ? SING CB HB2 ? ? SING CG CD1 ? ? SING CG CD2 ? ? SING CG HG ? ? SING CD1 HD11 ? ? SING CD1 HD12 ? ? SING CD1 HD13 ? ? SING CD2 HD21 ? ? SING CD2 HD22 ? ? SING CD2 HD23 ? ? SING OXT HXT ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $entity_1 'Trichoderma pseudokoningii' 317029 Eukaryota Fungi Trichoderma pseudokoningii 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 $entity_1 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type micelle _Details '1.9 mM Harzianin HK VI, 185 mM U-98% 2H DPC, 90 % H2O, 10% U-99% 2H D2O, 0.1 mM DSS, 90% H2O/10% D2O.' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling D2O 10 % 'U-99% 2H' DPC 185 mM 'U-98% 2H' DSS 0.1 mM 'natural abundance' H2O 90 % 'natural abundance' $entity_1 0.9 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name CYANA _Version 2.1 loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task 'structure calculation' stop_ _Details . save_ save_software_2 _Saveframe_category software _Name Molmol _Version . loop_ _Vendor _Address _Electronic_address 'Koradi, Billeter and Wuthrich' . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ save_software_3 _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_software_4 _Saveframe_category software _Name TALOS+ _Version . loop_ _Vendor _Address _Electronic_address 'Cornilescu, Delaglio and Bax' . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ save_software_5 _Saveframe_category software _Name TOPSPIN _Version . loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection processing stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details 'equipped with a cryoprobe' save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_COSY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H 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_ save_2D_1H-13C_HSQC_aliphatic_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $sample_1 save_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 0 . mM pH 7 . pH pressure 1 . atm temperature 298 . K stop_ save_ #################### # NMR parameters # #################### ############################## # Assigned chemical shifts # ############################## ################################ # Chemical shift referencing # ################################ save_chem_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 DSS C 13 'methyl protons' ppm 0.000 internal indirect . . . 0.25144953 DSS H 1 'methyl protons' ppm 0.000 internal direct . . . 1.0 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_chemical_shifts_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H COSY' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' '2D 1H-13C HSQC aliphatic' stop_ loop_ _Sample_label $sample_1 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name entity_1 _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 ACE H1 H 2.034 0.003 1 2 1 1 ACE H2 H 2.034 0.003 1 3 1 1 ACE H3 H 2.034 0.003 1 4 1 1 ACE CH3 C 25.411 0.000 1 5 2 2 AIB H H 9.046 0.004 1 6 2 2 AIB CB1 C 26.098 0.000 1 7 2 2 AIB CB2 C 28.883 0.000 1 8 2 2 AIB HB11 H 1.406 0.007 1 9 2 2 AIB HB12 H 1.406 0.007 1 10 2 2 AIB HB13 H 1.406 0.007 1 11 2 2 AIB HB21 H 1.434 0.005 1 12 2 2 AIB HB22 H 1.434 0.005 1 13 2 2 AIB HB23 H 1.434 0.005 1 14 3 3 ASN H H 8.668 0.003 1 15 3 3 ASN HA H 4.306 0.005 1 16 3 3 ASN HB2 H 2.791 0.003 2 17 3 3 ASN HB3 H 2.791 0.003 2 18 3 3 ASN HD21 H 6.880 0.003 2 19 3 3 ASN HD22 H 7.675 0.003 2 20 3 3 ASN CA C 55.654 0.000 1 21 3 3 ASN CB C 37.963 0.000 1 22 4 4 ILE H H 7.917 0.003 1 23 4 4 ILE HA H 3.968 0.003 1 24 4 4 ILE HB H 2.060 0.004 1 25 4 4 ILE HG12 H 1.262 0.005 2 26 4 4 ILE HG13 H 1.573 0.003 2 27 4 4 ILE HG2 H 0.913 0.002 1 28 4 4 ILE HD1 H 0.894 0.005 1 29 4 4 ILE CA C 62.837 0.000 1 30 4 4 ILE CB C 38.277 0.000 1 31 4 4 ILE CG1 C 28.421 0.001 1 32 4 4 ILE CG2 C 17.918 0.000 1 33 4 4 ILE CD1 C 13.295 0.000 1 34 5 5 ILE H H 7.336 0.004 1 35 5 5 ILE HA H 4.120 0.004 1 36 5 5 ILE HB H 1.924 0.003 1 37 5 5 ILE HG12 H 1.302 0.003 2 38 5 5 ILE HG13 H 1.558 0.003 2 39 5 5 ILE HG2 H 0.896 0.004 1 40 5 5 ILE HD1 H 0.788 0.004 1 41 5 5 ILE CA C 62.200 0.000 1 42 5 5 ILE CB C 38.761 0.000 1 43 5 5 ILE CG1 C 28.308 0.008 1 44 5 5 ILE CG2 C 17.996 0.000 1 45 5 5 ILE CD1 C 12.279 0.000 1 46 6 6 AIB H H 9.082 0.003 1 47 6 6 AIB CB1 C 25.959 0.000 1 48 6 6 AIB CB2 C 22.207 0.000 1 49 6 6 AIB HB11 H 1.406 0.006 1 50 6 6 AIB HB12 H 1.406 0.006 1 51 6 6 AIB HB13 H 1.406 0.006 1 52 6 6 AIB HB21 H 1.713 0.004 1 53 6 6 AIB HB22 H 1.713 0.004 1 54 6 6 AIB HB23 H 1.713 0.004 1 55 7 7 PRO HA H 4.490 0.006 1 56 7 7 PRO HB2 H 1.804 0.003 2 57 7 7 PRO HB3 H 2.372 0.004 2 58 7 7 PRO HG2 H 1.974 0.003 2 59 7 7 PRO HG3 H 1.974 0.003 2 60 7 7 PRO HD2 H 3.379 0.004 2 61 7 7 PRO HD3 H 3.819 0.004 2 62 7 7 PRO CB C 31.352 0.006 1 63 7 7 PRO CG C 28.712 0.000 1 64 7 7 PRO CD C 53.046 0.000 1 65 8 8 LEU H H 7.529 0.004 1 66 8 8 LEU HA H 4.150 0.005 1 67 8 8 LEU HB2 H 1.576 0.004 2 68 8 8 LEU HB3 H 1.918 0.003 2 69 8 8 LEU HG H 1.873 0.002 1 70 8 8 LEU HD1 H 0.910 0.004 2 71 8 8 LEU HD2 H 0.989 0.004 2 72 8 8 LEU CA C 56.650 0.000 1 73 8 8 LEU CB C 42.181 0.000 1 74 8 8 LEU CG C 27.446 0.000 1 75 8 8 LEU CD1 C 23.320 0.000 1 76 8 8 LEU CD2 C 26.144 0.000 1 77 9 9 LEU H H 6.955 0.004 1 78 9 9 LEU HA H 4.401 0.006 1 79 9 9 LEU HB2 H 1.618 0.006 2 80 9 9 LEU HB3 H 1.687 0.006 2 81 9 9 LEU HG H 1.659 0.007 1 82 9 9 LEU HD1 H 0.807 0.002 2 83 9 9 LEU HD2 H 0.848 0.004 2 84 9 9 LEU CA C 54.159 0.000 1 85 9 9 LEU CB C 42.725 0.009 1 86 9 9 LEU CG C 27.442 0.000 1 87 9 9 LEU CD1 C 23.348 0.000 1 88 9 9 LEU CD2 C 25.953 0.000 1 89 10 10 AIB H H 7.448 0.003 1 90 10 10 AIB CB1 C 28.324 0.000 1 91 10 10 AIB CB2 C 25.970 0.000 1 92 10 10 AIB HB11 H 1.438 0.003 1 93 10 10 AIB HB12 H 1.438 0.003 1 94 10 10 AIB HB13 H 1.438 0.003 1 95 10 10 AIB HB21 H 1.472 0.004 1 96 10 10 AIB HB22 H 1.472 0.004 1 97 10 10 AIB HB23 H 1.472 0.004 1 98 11 11 PRO HA H 4.487 0.005 1 99 11 11 PRO HB2 H 1.704 0.004 2 100 11 11 PRO HB3 H 2.354 0.004 2 101 11 11 PRO HG2 H 1.888 0.003 2 102 11 11 PRO HG3 H 1.957 0.004 2 103 11 11 PRO HD2 H 3.282 0.003 2 104 11 11 PRO HD3 H 3.774 0.004 2 105 11 11 PRO CB C 31.980 0.000 1 106 11 11 PRO CG C 28.310 0.007 1 107 11 11 PRO CD C 52.172 0.000 1 108 12 12 DCL C C 68.011 0.000 1 109 12 12 DCL CA C 53.103 0.000 1 110 12 12 DCL CB C 41.888 0.002 1 111 12 12 DCL CD1 C 24.270 0.000 1 112 12 12 DCL CD2 C 26.495 0.000 1 113 12 12 DCL CG C 27.562 0.000 1 114 12 12 DCL HA H 3.967 0.003 1 115 12 12 DCL HB1 H 3.439 0.002 2 116 12 12 DCL HB2 H 3.477 0.003 2 117 12 12 DCL HC1 H 1.532 0.004 2 118 12 12 DCL HC2 H 1.221 0.003 2 119 12 12 DCL HD11 H 0.861 0.003 2 120 12 12 DCL HD12 H 0.861 0.003 2 121 12 12 DCL HD13 H 0.861 0.003 2 122 12 12 DCL HD21 H 0.931 0.004 2 123 12 12 DCL HD22 H 0.931 0.004 2 124 12 12 DCL HD23 H 0.931 0.004 2 125 12 12 DCL HG H 1.596 0.005 1 126 12 12 DCL HN1 H 7.587 0.004 1 stop_ save_