data_18722 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; High resolution NMR solution structure of a symmetrical theta-defensin, BTD-2. ; _BMRB_accession_number 18722 _BMRB_flat_file_name bmr18722.str _Entry_type original _Submission_date 2012-09-18 _Accession_date 2012-09-18 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details 'Head-to-tail (Arg-Gly) cyclic peptide' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Conibear Anne C. . 2 Rosengren 'K. Johan' . . 3 Harvey Peta J. . 4 Craik David J. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 98 "13C chemical shifts" 54 "15N chemical shifts" 16 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2013-02-18 update BMRB 'update entry citation' 2012-11-27 original author 'original release' stop_ loop_ _Related_BMRB_accession_number _Relationship 18723 'theta-defensin RTD-1' stop_ save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title 'Structural Characterization of the Cyclic Cystine Ladder Motif of -Defensins.' _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 23148585 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Conibear Anne C. . 2 Rosengren 'K. Johan' . . 3 Harvey Peta J. . 4 Craik David J. . stop_ _Journal_abbreviation Biochemistry _Journal_name_full Biochemistry _Journal_volume 51 _Journal_issue 48 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 9718 _Page_last 9726 _Year 2012 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name BTD-2 _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label BTD-2 $BTD-2 stop_ _System_molecular_weight . _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_BTD-2 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common BTD-2 _Molecular_mass 2090.649 _Mol_thiol_state 'all disulfied bond' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 18 _Mol_residue_sequence GVCRCVCRRGVCRCVCRR loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 GLY 2 2 VAL 3 3 CYS 4 4 ARG 5 5 CYS 6 6 VAL 7 7 CYS 8 8 ARG 9 9 ARG 10 10 GLY 11 11 VAL 12 12 CYS 13 13 ARG 14 14 CYS 15 15 VAL 16 16 CYS 17 17 ARG 18 18 ARG stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date 2014-11-09 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 PDB 2LYE "High Resolution Nmr Solution Structure Of A Symmetrical Theta- Defensin, Btd-2" 100.00 18 100.00 100.00 2.38e+00 stop_ save_ ######################################## # Molecular bond linkage definitions # ######################################## save_crosslink_bonds _Saveframe_category crosslink_bonds loop_ _Bond_order _Bond_type _Atom_one_mol_system_component_name _Atom_one_residue_seq_code _Atom_one_residue_label _Atom_one_atom_name _Atom_two_mol_system_component_name _Atom_two_residue_seq_code _Atom_two_residue_label _Atom_two_atom_name single disulfide BTD-2 3 CYS SG BTD-2 16 CYS SG single disulfide BTD-2 5 CYS SG BTD-2 14 CYS SG single disulfide BTD-2 7 CYS SG BTD-2 12 CYS SG stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $BTD-2 'Olive baboon' 9555 Eukaryota Metazoa Papio anubis 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 _Details $BTD-2 'chemical synthesis' . . . . . 'Solid phase peptide synthesis' stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '0.8 mM, pH 6' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $BTD-2 0.8 mM 'natural abundance' H2O 90 % 'natural abundance' D2O 10 % 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details '0.9 mM, pH 6' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $BTD-2 0.9 mM 'natural abundance' D2O 100 % 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CcpNmr _Saveframe_category software _Name CcpNmr _Version 2.1 loop_ _Vendor _Address _Electronic_address CCPN . http://www.ccpn.ac.uk/software/analysis stop_ loop_ _Task 'data analysis' 'chemical shift assignment' 'peak picking' stop_ _Details . save_ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version 2.1 loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection processing stop_ _Details . save_ save_CYANA _Saveframe_category software _Name CYANA _Version 3.0 loop_ _Vendor _Address _Electronic_address 'Guntert, Mumenthaler and Wuthrich' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ save_CNS _Saveframe_category software _Name CNS _Version 2.1 loop_ _Vendor _Address _Electronic_address 'Brunger, Adams, Clore, Gros, Nilges and Read' . . stop_ loop_ _Task refinement stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 500 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ save_spectrometer_3 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 900 _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_2 save_ save_2D_DQF-COSY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $sample_1 save_ save_2D_1H-1H_ECOSY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H ECOSY' _Sample_label $sample_2 save_ save_2D_1H-15N_HSQC_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _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 temperature 298 . K pH 6 . pH pressure 1 . atm 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 DSS H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 DSS C 13 'methyl protons' ppm 0.00 internal indirect . . . 0.251449530 water N 15 protons ppm 0.00 na indirect . . . -0.101363 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' '2D 1H-15N HSQC' stop_ loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name BTD-2 _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 GLY HA2 H 3.603 0.010 1 2 1 1 GLY HA3 H 4.179 0.010 1 3 1 1 GLY H H 8.693 0.010 1 4 1 1 GLY CA C 45.257 0.010 1 5 1 1 GLY N N 104.380 0.010 1 6 2 2 VAL H H 7.814 0.010 1 7 2 2 VAL HA H 4.283 0.010 1 8 2 2 VAL HB H 2.141 0.010 1 9 2 2 VAL HG1 H 0.942 0.010 1 10 2 2 VAL HG2 H 0.942 0.010 1 11 2 2 VAL CA C 61.860 0.010 1 12 2 2 VAL CB C 33.351 0.010 1 13 2 2 VAL CG1 C 18.061 0.010 1 14 2 2 VAL CG2 C 18.061 0.010 1 15 2 2 VAL N N 121.870 0.010 1 16 3 3 CYS H H 9.114 0.010 1 17 3 3 CYS HA H 5.454 0.010 1 18 3 3 CYS HB2 H 2.627 0.010 1 19 3 3 CYS HB3 H 3.026 0.010 1 20 3 3 CYS CA C 55.354 0.010 1 21 3 3 CYS CB C 47.049 0.010 1 22 3 3 CYS N N 126.480 0.010 1 23 4 4 ARG H H 8.733 0.010 1 24 4 4 ARG HA H 4.691 0.010 1 25 4 4 ARG HB2 H 1.830 0.010 1 26 4 4 ARG HB3 H 1.830 0.010 1 27 4 4 ARG HG2 H 1.669 0.010 1 28 4 4 ARG HG3 H 1.570 0.010 1 29 4 4 ARG HD2 H 3.225 0.010 1 30 4 4 ARG HD3 H 3.225 0.010 1 31 4 4 ARG CA C 55.050 0.010 1 32 4 4 ARG CB C 32.296 0.010 1 33 4 4 ARG CG C 27.514 0.010 1 34 4 4 ARG CD C 43.360 0.010 1 35 4 4 ARG N N 123.800 0.010 1 36 5 5 CYS H H 9.180 0.010 1 37 5 5 CYS HA H 5.566 0.010 1 38 5 5 CYS HB2 H 2.624 0.010 1 39 5 5 CYS HB3 H 3.110 0.010 1 40 5 5 CYS CA C 55.556 0.010 1 41 5 5 CYS CB C 48.567 0.010 1 42 5 5 CYS N N 124.240 0.010 1 43 6 6 VAL H H 8.703 0.010 1 44 6 6 VAL HA H 4.324 0.010 1 45 6 6 VAL HB H 2.042 0.010 1 46 6 6 VAL HG1 H 0.960 0.010 1 47 6 6 VAL HG2 H 0.960 0.010 1 48 6 6 VAL CA C 61.810 0.010 1 49 6 6 VAL CB C 34.339 0.010 1 50 6 6 VAL CG1 C 20.693 0.010 1 51 6 6 VAL CG2 C 20.693 0.010 1 52 6 6 VAL N N 123.340 0.010 1 53 7 7 CYS H H 9.150 0.010 1 54 7 7 CYS HA H 5.597 0.010 1 55 7 7 CYS HB2 H 2.645 0.010 1 56 7 7 CYS HB3 H 3.117 0.010 1 57 7 7 CYS CA C 55.286 0.010 1 58 7 7 CYS CB C 48.201 0.010 1 59 7 7 CYS N N 127.520 0.010 1 60 8 8 ARG H H 8.696 0.010 1 61 8 8 ARG HA H 4.523 0.010 1 62 8 8 ARG HB2 H 1.782 0.010 1 63 8 8 ARG HB3 H 1.782 0.010 1 64 8 8 ARG HG2 H 1.643 0.010 1 65 8 8 ARG HG3 H 1.536 0.010 1 66 8 8 ARG HD2 H 3.224 0.010 1 67 8 8 ARG HD3 H 3.224 0.010 1 68 8 8 ARG CA C 55.508 0.010 1 69 8 8 ARG CB C 32.715 0.010 1 70 8 8 ARG CG C 27.164 0.010 1 71 8 8 ARG CD C 43.226 0.010 1 72 8 8 ARG N N 123.350 0.010 1 73 9 9 ARG H H 9.600 0.010 1 74 9 9 ARG HA H 3.920 0.010 1 75 9 9 ARG HB2 H 2.089 0.010 1 76 9 9 ARG HB3 H 1.833 0.010 1 77 9 9 ARG HG2 H 1.634 0.010 1 78 9 9 ARG HG3 H 1.634 0.010 1 79 9 9 ARG HD2 H 3.230 0.010 1 80 9 9 ARG HD3 H 3.230 0.010 1 81 9 9 ARG CA C 56.983 0.010 1 82 9 9 ARG CB C 28.096 0.010 1 83 9 9 ARG CG C 27.886 0.010 1 84 9 9 ARG CD C 43.080 0.010 1 85 10 10 GLY H H 8.693 0.010 1 86 10 10 GLY HA2 H 3.603 0.010 1 87 10 10 GLY HA3 H 4.179 0.010 1 88 10 10 GLY CA C 45.257 0.010 1 89 10 10 GLY N N 104.380 0.010 1 90 11 11 VAL H H 7.814 0.010 1 91 11 11 VAL HA H 4.283 0.010 1 92 11 11 VAL HB H 2.141 0.010 1 93 11 11 VAL HG1 H 0.942 0.010 1 94 11 11 VAL HG2 H 0.942 0.010 1 95 11 11 VAL CA C 61.860 0.010 1 96 11 11 VAL CB C 33.351 0.010 1 97 11 11 VAL CG1 C 18.061 0.010 1 98 11 11 VAL CG2 C 18.061 0.010 1 99 11 11 VAL N N 121.870 0.010 1 100 12 12 CYS H H 9.114 0.010 1 101 12 12 CYS HA H 5.454 0.010 1 102 12 12 CYS HB2 H 2.627 0.010 1 103 12 12 CYS HB3 H 3.026 0.010 1 104 12 12 CYS CA C 55.354 0.010 1 105 12 12 CYS CB C 47.049 0.010 1 106 12 12 CYS N N 126.480 0.010 1 107 13 13 ARG H H 8.733 0.010 1 108 13 13 ARG HA H 4.691 0.010 1 109 13 13 ARG HB2 H 1.830 0.010 1 110 13 13 ARG HB3 H 1.830 0.010 1 111 13 13 ARG HG2 H 1.669 0.010 1 112 13 13 ARG HG3 H 1.570 0.010 1 113 13 13 ARG HD2 H 3.225 0.010 1 114 13 13 ARG HD3 H 3.225 0.010 1 115 13 13 ARG CA C 55.050 0.010 1 116 13 13 ARG CB C 32.296 0.010 1 117 13 13 ARG CG C 27.514 0.010 1 118 13 13 ARG CD C 43.360 0.010 1 119 13 13 ARG N N 123.800 0.010 1 120 14 14 CYS H H 9.180 0.010 1 121 14 14 CYS HA H 5.566 0.010 1 122 14 14 CYS HB2 H 2.624 0.010 1 123 14 14 CYS HB3 H 3.110 0.010 1 124 14 14 CYS CA C 55.556 0.010 1 125 14 14 CYS CB C 48.567 0.010 1 126 14 14 CYS N N 124.240 0.010 1 127 15 15 VAL H H 8.703 0.010 1 128 15 15 VAL HA H 4.324 0.010 1 129 15 15 VAL HB H 2.042 0.010 1 130 15 15 VAL HG1 H 0.960 0.010 1 131 15 15 VAL HG2 H 0.960 0.010 1 132 15 15 VAL CA C 61.810 0.010 1 133 15 15 VAL CB C 34.339 0.010 1 134 15 15 VAL CG1 C 20.693 0.010 1 135 15 15 VAL CG2 C 20.693 0.010 1 136 15 15 VAL N N 123.340 0.010 1 137 16 16 CYS H H 9.150 0.010 1 138 16 16 CYS HA H 5.597 0.010 1 139 16 16 CYS HB2 H 2.645 0.010 1 140 16 16 CYS HB3 H 3.117 0.010 1 141 16 16 CYS CA C 55.286 0.010 1 142 16 16 CYS CB C 48.201 0.010 1 143 16 16 CYS N N 127.520 0.010 1 144 17 17 ARG H H 8.696 0.010 1 145 17 17 ARG HA H 4.523 0.010 1 146 17 17 ARG HB2 H 1.782 0.010 1 147 17 17 ARG HB3 H 1.782 0.010 1 148 17 17 ARG HG2 H 1.643 0.010 1 149 17 17 ARG HG3 H 1.536 0.010 1 150 17 17 ARG HD2 H 3.224 0.010 1 151 17 17 ARG HD3 H 3.224 0.010 1 152 17 17 ARG CA C 55.508 0.010 1 153 17 17 ARG CB C 32.715 0.010 1 154 17 17 ARG CG C 27.164 0.010 1 155 17 17 ARG CD C 43.226 0.010 1 156 17 17 ARG N N 123.350 0.010 1 157 18 18 ARG H H 9.600 0.010 1 158 18 18 ARG HA H 3.920 0.010 1 159 18 18 ARG HB2 H 2.089 0.010 1 160 18 18 ARG HB3 H 1.833 0.010 1 161 18 18 ARG HG2 H 1.634 0.010 1 162 18 18 ARG HG3 H 1.634 0.010 1 163 18 18 ARG HD2 H 3.230 0.010 1 164 18 18 ARG HD3 H 3.230 0.010 1 165 18 18 ARG CA C 56.983 0.010 1 166 18 18 ARG CB C 28.096 0.010 1 167 18 18 ARG CG C 27.886 0.010 1 168 18 18 ARG CD C 43.080 0.010 1 stop_ save_