data_30213 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Ocellatin-F1, solution structure in TFE by NMR spectroscopy ; _BMRB_accession_number 30213 _BMRB_flat_file_name bmr30213.str _Entry_type original _Submission_date 2016-12-18 _Accession_date 2016-12-18 _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 Gusmao K. A.G. . 2 'dos Santos' D. M. . 3 Santos V. M. . 4 Pilo-Veloso D. . . 5 'de Lima' M. E. . 6 Resende J. M. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 132 "13C chemical shifts" 78 "15N chemical shifts" 24 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2017-03-24 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 30211 'Ocellatin LB1' 30212 'Ocellatin LB2' 30214 'Ocellatin LB1' 30215 Ocellatin-LB2 30216 'Ocellatin K1 (26)' 30217 'Ocellatin LB1' 30218 'Ocellatin LB2' 30219 'Ocellatin F1' stop_ _Original_release_date 2017-03-22 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; Ocellatin-F1 ; _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 Gusmao K. A.G. . 2 'dos Santos' D. M. . 3 Santos V. M. . 4 Pilo-Veloso D. . . 5 'de Lima' M. E. . 6 Resende J. M. . 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_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name Ocellatin-F1 _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 2552.089 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 26 _Mol_residue_sequence ; GVVDILKGAAKDIAGHLASK VMNKLX ; loop_ _Residue_seq_code _Residue_label 1 GLY 2 VAL 3 VAL 4 ASP 5 ILE 6 LEU 7 LYS 8 GLY 9 ALA 10 ALA 11 LYS 12 ASP 13 ILE 14 ALA 15 GLY 16 HIS 17 LEU 18 ALA 19 SER 20 LYS 21 VAL 22 MET 23 ASN 24 LYS 25 LEU 26 NH2 stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_NH2 _Saveframe_category polymer_residue _Mol_type NON-POLYMER _Name_common 'AMINO GROUP' _BMRB_code NH2 _PDB_code NH2 _Standard_residue_derivative . _Molecular_mass 16.023 _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 . ? 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 $entity_1 'frogs and toads' 326590 Eukaryota Metazoa Leptodactylus labyrinthicus 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 solution _Details ; 2.0 mM Ocellatin-F1, 1.0 mM DSS, 20 mM potassium phosphate, 60 % d2 TFE, 40 % H2O, trifluoroethanol/water. ; loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling DSS 1.0 mM 'natural abundance' H2O 40 % 'natural abundance' $entity_1 2.0 mM 'natural abundance' TFE 60 % [U-2H] 'potassium phosphate' 20 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _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_2 _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_software_3 _Saveframe_category software _Name NMRView _Version . loop_ _Vendor _Address _Electronic_address 'Johnson, One Moon Scientific' . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ save_software_4 _Saveframe_category software _Name Procheck _Version . loop_ _Vendor _Address _Electronic_address 'Laskowski, MacArthur, Smith, Jones, Hutchinson, Morris, Moss and Thornton' . . stop_ loop_ _Task 'data analysis' stop_ _Details . save_ save_software_5 _Saveframe_category software _Name X-PLOR_NIH _Version 2.27 loop_ _Vendor _Address _Electronic_address 'Schwieters, Kuszewski, Tjandra and Clore' . . stop_ loop_ _Task 'geometry optimization' refinement 'structure calculation' stop_ _Details . save_ save_software_6 _Saveframe_category software _Name xwinnmr _Version . loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AvanceIII _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_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-15N_HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $sample_1 save_ save_2D_1H-13C_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C 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 pH 7 . pH pressure 1 . atm temperature 293.15 . 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 TOCSY' '2D 1H-1H NOESY' '2D 1H-15N HSQC' '2D 1H-13C HSQC' 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 GLY HA2 H 4.110 . . 2 1 1 GLY HA3 H 3.957 . . 3 1 1 GLY CA C 43.414 . . 4 2 2 VAL H H 8.136 . . 5 2 2 VAL HA H 3.860 . . 6 2 2 VAL HB H 2.112 . . 7 2 2 VAL HG1 H 1.116 . . 8 2 2 VAL HG2 H 1.036 . . 9 2 2 VAL CA C 66.317 . . 10 2 2 VAL CB C 32.563 . . 11 2 2 VAL CG1 C 21.121 . . 12 2 2 VAL CG2 C 20.041 . . 13 3 3 VAL H H 8.138 . . 14 3 3 VAL HA H 3.787 . . 15 3 3 VAL HB H 2.110 . . 16 3 3 VAL HG1 H 1.078 . . 17 3 3 VAL HG2 H 0.996 . . 18 3 3 VAL CA C 66.067 . . 19 3 3 VAL CB C 32.029 . . 20 3 3 VAL CG1 C 21.852 . . 21 3 3 VAL CG2 C 20.702 . . 22 3 3 VAL N N 117.918 . . 23 4 4 ASP H H 7.424 . . 24 4 4 ASP HA H 4.391 . . 25 4 4 ASP HB2 H 2.845 . . 26 4 4 ASP HB3 H 2.754 . . 27 4 4 ASP CA C 57.323 . . 28 4 4 ASP CB C 41.028 . . 29 4 4 ASP N N 114.356 . . 30 5 5 ILE H H 7.614 . . 31 5 5 ILE HA H 3.863 . . 32 5 5 ILE HB H 2.173 . . 33 5 5 ILE HG12 H 1.733 . . 34 5 5 ILE HG13 H 1.247 . . 35 5 5 ILE HG2 H 0.977 . . 36 5 5 ILE HD1 H 0.910 . . 37 5 5 ILE CA C 64.384 . . 38 5 5 ILE CB C 37.867 . . 39 5 5 ILE CG1 C 28.121 . . 40 5 5 ILE CG2 C 16.331 . . 41 5 5 ILE CD1 C 12.386 . . 42 5 5 ILE N N 120.520 . . 43 6 6 LEU H H 8.106 . . 44 6 6 LEU HA H 4.151 . . 45 6 6 LEU HB2 H 1.946 . . 46 6 6 LEU HB3 H 1.596 . . 47 6 6 LEU HG H 1.892 . . 48 6 6 LEU HD1 H 0.923 . . 49 6 6 LEU HD2 H 0.890 . . 50 6 6 LEU CA C 58.052 . . 51 6 6 LEU CB C 41.532 . . 52 6 6 LEU CG C 26.720 . . 53 6 6 LEU CD1 C 22.765 . . 54 6 6 LEU CD2 C 21.916 . . 55 6 6 LEU N N 120.404 . . 56 7 7 LYS H H 8.437 . . 57 7 7 LYS HA H 4.085 . . 58 7 7 LYS HB2 H 1.979 . . 59 7 7 LYS HB3 H 1.928 . . 60 7 7 LYS HG2 H 1.767 . . 61 7 7 LYS HG3 H 1.478 . . 62 7 7 LYS HD2 H 1.753 . . 63 7 7 LYS HE2 H 3.040 . . 64 7 7 LYS HE3 H 2.968 . . 65 7 7 LYS CA C 59.600 . . 66 7 7 LYS CB C 32.686 . . 67 7 7 LYS CG C 25.517 . . 68 7 7 LYS CD C 29.357 . . 69 7 7 LYS CE C 42.049 . . 70 7 7 LYS N N 117.855 . . 71 8 8 GLY H H 7.999 . . 72 8 8 GLY HA2 H 3.941 . . 73 8 8 GLY HA3 H 3.868 . . 74 8 8 GLY CA C 46.812 . . 75 8 8 GLY N N 106.100 . . 76 9 9 ALA H H 8.352 . . 77 9 9 ALA HA H 4.336 . . 78 9 9 ALA HB H 1.568 . . 79 9 9 ALA CA C 54.783 . . 80 9 9 ALA CB C 17.874 . . 81 9 9 ALA N N 125.131 . . 82 10 10 ALA H H 8.208 . . 83 10 10 ALA HA H 4.127 . . 84 10 10 ALA HB H 1.568 . . 85 10 10 ALA CA C 55.171 . . 86 10 10 ALA CB C 17.629 . . 87 10 10 ALA N N 119.854 . . 88 11 11 LYS H H 7.900 . . 89 11 11 LYS HA H 4.127 . . 90 11 11 LYS HB2 H 2.022 . . 91 11 11 LYS HB3 H 1.918 . . 92 11 11 LYS HG2 H 1.569 . . 93 11 11 LYS HD2 H 1.757 . . 94 11 11 LYS HD3 H 1.682 . . 95 11 11 LYS HE2 H 3.044 . . 96 11 11 LYS HE3 H 2.956 . . 97 11 11 LYS CA C 59.192 . . 98 11 11 LYS CB C 32.170 . . 99 11 11 LYS CG C 24.718 . . 100 11 11 LYS CD C 28.762 . . 101 11 11 LYS CE C 42.173 . . 102 11 11 LYS N N 117.074 . . 103 12 12 ASP H H 8.052 . . 104 12 12 ASP HA H 4.639 . . 105 12 12 ASP HB2 H 2.934 . . 106 12 12 ASP HB3 H 2.841 . . 107 12 12 ASP CA C 56.915 . . 108 12 12 ASP CB C 40.750 . . 109 12 12 ASP N N 121.195 . . 110 13 13 ILE H H 8.511 . . 111 13 13 ILE HA H 3.826 . . 112 13 13 ILE HB H 1.992 . . 113 13 13 ILE HG12 H 1.843 . . 114 13 13 ILE HG13 H 1.165 . . 115 13 13 ILE HG2 H 1.001 . . 116 13 13 ILE HD1 H 0.894 . . 117 13 13 ILE CA C 65.463 . . 118 13 13 ILE CB C 38.309 . . 119 13 13 ILE CG1 C 28.923 . . 120 13 13 ILE CG2 C 16.449 . . 121 13 13 ILE CD1 C 12.320 . . 122 13 13 ILE N N 122.797 . . 123 14 14 ALA H H 8.421 . . 124 14 14 ALA HA H 4.127 . . 125 14 14 ALA HB H 1.570 . . 126 14 14 ALA CA C 55.631 . . 127 14 14 ALA CB C 17.643 . . 128 14 14 ALA N N 122.025 . . 129 15 15 GLY H H 8.291 . . 130 15 15 GLY HA2 H 3.983 . . 131 15 15 GLY HA3 H 3.911 . . 132 15 15 GLY CA C 46.838 . . 133 15 15 GLY N N 103.974 . . 134 16 16 HIS H H 8.180 . . 135 16 16 HIS HA H 4.430 . . 136 16 16 HIS HB2 H 3.373 . . 137 16 16 HIS HD2 H 7.113 . . 138 16 16 HIS CA C 59.856 . . 139 16 16 HIS CB C 28.985 . . 140 16 16 HIS N N 121.600 . . 141 17 17 LEU H H 8.665 . . 142 17 17 LEU HA H 4.127 . . 143 17 17 LEU HB2 H 1.908 . . 144 17 17 LEU HB3 H 1.697 . . 145 17 17 LEU HG H 1.862 . . 146 17 17 LEU HD1 H 0.952 . . 147 17 17 LEU HD2 H 0.929 . . 148 17 17 LEU CA C 58.365 . . 149 17 17 LEU CB C 41.607 . . 150 17 17 LEU CG C 26.825 . . 151 17 17 LEU CD1 C 24.003 . . 152 17 17 LEU CD2 C 24.636 . . 153 17 17 LEU N N 121.652 . . 154 18 18 ALA H H 8.576 . . 155 18 18 ALA HA H 4.076 . . 156 18 18 ALA HB H 1.553 . . 157 18 18 ALA CA C 55.444 . . 158 18 18 ALA CB C 17.531 . . 159 18 18 ALA N N 120.492 . . 160 19 19 SER H H 7.892 . . 161 19 19 SER HA H 4.199 . . 162 19 19 SER HB2 H 4.076 . . 163 19 19 SER HB3 H 4.031 . . 164 19 19 SER CA C 61.741 . . 165 19 19 SER CB C 62.966 . . 166 19 19 SER N N 111.526 . . 167 20 20 LYS H H 7.842 . . 168 20 20 LYS HA H 4.192 . . 169 20 20 LYS HB2 H 2.104 . . 170 20 20 LYS HB3 H 2.006 . . 171 20 20 LYS HG2 H 1.606 . . 172 20 20 LYS HG3 H 1.491 . . 173 20 20 LYS HD2 H 1.706 . . 174 20 20 LYS HD3 H 1.616 . . 175 20 20 LYS HE2 H 2.967 . . 176 20 20 LYS HE3 H 2.868 . . 177 20 20 LYS CA C 59.060 . . 178 20 20 LYS CB C 32.501 . . 179 20 20 LYS CG C 24.762 . . 180 20 20 LYS CD C 28.967 . . 181 20 20 LYS N N 122.371 . . 182 21 21 VAL H H 8.177 . . 183 21 21 VAL HA H 3.740 . . 184 21 21 VAL HB H 2.236 . . 185 21 21 VAL HG1 H 1.079 . . 186 21 21 VAL HG2 H 0.983 . . 187 21 21 VAL CA C 66.365 . . 188 21 21 VAL CB C 32.102 . . 189 21 21 VAL CG1 C 21.673 . . 190 21 21 VAL CG2 C 20.657 . . 191 21 21 VAL N N 119.526 . . 192 22 22 MET H H 8.460 . . 193 22 22 MET HA H 4.262 . . 194 22 22 MET HB2 H 2.222 . . 195 22 22 MET HB3 H 2.131 . . 196 22 22 MET HG2 H 2.763 . . 197 22 22 MET HG3 H 2.626 . . 198 22 22 MET CA C 58.119 . . 199 22 22 MET CB C 32.052 . . 200 22 22 MET CG C 32.271 . . 201 22 22 MET N N 117.466 . . 202 23 23 ASN H H 7.970 . . 203 23 23 ASN HA H 4.583 . . 204 23 23 ASN HB2 H 2.964 . . 205 23 23 ASN HB3 H 2.865 . . 206 23 23 ASN HD21 H 7.651 . . 207 23 23 ASN HD22 H 6.730 . . 208 23 23 ASN CA C 55.430 . . 209 23 23 ASN CB C 39.086 . . 210 23 23 ASN N N 116.363 . . 211 23 23 ASN ND2 N 111.555 . . 212 24 24 LYS H H 7.958 . . 213 24 24 LYS HA H 4.280 . . 214 24 24 LYS HB2 H 2.020 . . 215 24 24 LYS HB3 H 1.915 . . 216 24 24 LYS HG2 H 1.745 . . 217 24 24 LYS HG3 H 1.683 . . 218 24 24 LYS HD2 H 1.731 . . 219 24 24 LYS CA C 57.628 . . 220 24 24 LYS CB C 32.645 . . 221 24 24 LYS CG C 24.789 . . 222 24 24 LYS CD C 29.742 . . 223 24 24 LYS N N 119.461 . . 224 25 25 LEU H H 8.066 . . 225 25 25 LEU HA H 4.278 . . 226 25 25 LEU HB2 H 1.836 . . 227 25 25 LEU HB3 H 1.624 . . 228 25 25 LEU HD1 H 0.935 . . 229 25 25 LEU HD2 H 0.894 . . 230 25 25 LEU CA C 55.804 . . 231 25 25 LEU CB C 42.552 . . 232 25 25 LEU CD1 C 24.642 . . 233 25 25 LEU CD2 C 21.804 . . 234 25 25 LEU N N 119.553 . . stop_ save_