data_26794 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR Assignment of L-Dfp6,D-Trp8-SRIF ; _BMRB_accession_number 26794 _BMRB_flat_file_name bmr26794.str _Entry_type original _Submission_date 2016-05-12 _Accession_date 2016-05-12 _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 Macias Maria J. . 2 Riera Antoni . . 3 Martin-Gago Pablo . . 4 Rol Alvaro . . 5 Martin-Malpartida Pau . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 82 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2016-08-31 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 26795 'NMR Assignment of L-Dfp7,D-Trp8-SRIF' 26796 'NMR Assignment of L-Dfp11,D-Trp8-SRIF' 26797 'NMR Assignment of L-Dfp6,L-Msa7,D-Trp8-SRIF' 26798 'NMR Assignment of L-Dfp11,L-Msa7,D-Trp8-SRIF' 26799 'NMR Assignment of L-Dfp6,L-Msa7,D-Trp8, L-Dfp11-SRIF' stop_ _Original_release_date 2016-08-31 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Peptide aromatic interactions modulated by fluorinated residues: Synthesis, structure and biological activity of Somatostatin analogs containing 3-(3',5'difluorophenyl)-alanine ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 27271737 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Martin-Gago Pablo . . 2 Rol Alvaro . . 3 Todorovski Toni . . 4 Aragon Eric . . 5 Martin-Malpartida Pau . . 6 Verdaguer Xavier . . 7 Valles-Miret Mariona . . 8 Fernandez-Carneado Jimena . . 9 Ponsati Berta . . 10 Macias Maria J. . 11 Riera Antoni . . stop_ _Journal_abbreviation 'Sci. Rep.' _Journal_volume 6 _Journal_issue . _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 27285 _Page_last 27285 _Year 2016 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name Assembly _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label L-Dfp6,D-Trp8-SRIF $L-Dfp6-D-Trp8-SRIF 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_L-Dfp6-D-Trp8-SRIF _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class protein _Name_common L-Dfp6,D-Trp8-SRIF _Molecular_mass . _Mol_thiol_state 'all disulfide bound' loop_ _Biological_function Hormone stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 14 _Mol_residue_sequence ; AGCKNXFXKTFTSC ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 ALA 2 2 GLY 3 3 CYS 4 4 LYS 5 5 ASN 6 6 WFP 7 7 PHE 8 8 DTR 9 9 LYS 10 10 THR 11 11 PHE 12 12 THR 13 13 SER 14 14 CYS stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_DTR _Saveframe_category polymer_residue _Mol_type 'D-PEPTIDE LINKING' _Name_common D-TRYPTOPHAN _BMRB_code DTR _PDB_code DTR _Standard_residue_derivative . _Molecular_mass 204.225 _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 . ? CB CB C . 0 . ? CG CG C . 0 . ? CD1 CD1 C . 0 . ? NE1 NE1 N . 0 . ? CE2 CE2 C . 0 . ? CZ2 CZ2 C . 0 . ? CH2 CH2 C . 0 . ? CZ3 CZ3 C . 0 . ? CE3 CE3 C . 0 . ? CD2 CD2 C . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? HN2 HN2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HD1 HD1 H . 0 . ? HE1 HE1 H . 0 . ? HZ2 HZ2 H . 0 . ? HH2 HH2 H . 0 . ? HZ3 HZ3 H . 0 . ? HE3 HE3 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 H ? ? SING N HN2 ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB CG ? ? SING CB HB2 ? ? SING CB HB3 ? ? DOUB CG CD1 ? ? SING CG CD2 ? ? SING CD1 NE1 ? ? SING CD1 HD1 ? ? SING NE1 CE2 ? ? SING NE1 HE1 ? ? DOUB CE2 CZ2 ? ? SING CE2 CD2 ? ? SING CZ2 CH2 ? ? SING CZ2 HZ2 ? ? DOUB CH2 CZ3 ? ? SING CH2 HH2 ? ? SING CZ3 CE3 ? ? SING CZ3 HZ3 ? ? DOUB CE3 CD2 ? ? SING CE3 HE3 ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? stop_ save_ save_chem_comp_WFP _Saveframe_category polymer_residue _Mol_type 'L-PEPTIDE LINKING' _Name_common 3,5-difluoro-L-phenylalanine _BMRB_code WFP _PDB_code WFP _Standard_residue_derivative . _Molecular_mass 201.170 _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 . ? N N N . 0 . ? O O O . 0 . ? F1 F1 F . 0 . ? F2 F2 F . 0 . ? CA CA C . 0 . ? CB CB C . 0 . ? CG CG C . 0 . ? CZ CZ C . 0 . ? CD1 CD1 C . 0 . ? CD2 CD2 C . 0 . ? CE1 CE1 C . 0 . ? CE2 CE2 C . 0 . ? OXT OXT O . 0 . ? H H H . 0 . ? H2 H2 H . 0 . ? HA HA H . 0 . ? HB2 HB2 H . 0 . ? HB3 HB3 H . 0 . ? HZ HZ H . 0 . ? HD1 HD1 H . 0 . ? HD2 HD2 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 DOUB C O ? ? SING C CA ? ? SING C OXT ? ? SING N CA ? ? SING F1 CE1 ? ? SING F2 CE2 ? ? SING CA CB ? ? SING CB CG ? ? DOUB CG CD1 ? ? SING CG CD2 ? ? DOUB CZ CE1 ? ? SING CZ CE2 ? ? SING CD1 CE1 ? ? DOUB CD2 CE2 ? ? SING N H ? ? SING N H2 ? ? SING CA HA ? ? SING CB HB2 ? ? SING CB HB3 ? ? SING CZ HZ ? ? SING CD1 HD1 ? ? SING CD2 HD2 ? ? 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 $L-Dfp6-D-Trp8-SRIF . . . . . . 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 $L-Dfp6-D-Trp8-SRIF 'chemical synthesis' . . . . . 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 $L-Dfp6-D-Trp8-SRIF 1 mM 'natural abundance' D2O 10 % '[U-100% 2H]' H2O 90 % 'natural abundance' 'sodium phosphate' 100 mM 'natural abundance' 'sodium chloride' 50 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_CNSSOLVE _Saveframe_category software _Name CNSSOLVE _Version . loop_ _Vendor _Address _Electronic_address 'Brunger, Adams, Clore, Gros, Nilges and Read' . . stop_ loop_ _Task 'structure solution' stop_ _Details . save_ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version . loop_ _Vendor _Address _Electronic_address 'Bruker Biospin' . . stop_ loop_ _Task collection stop_ _Details . save_ save_NMRPipe _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_CARA _Saveframe_category software _Name CARA _Version . loop_ _Vendor _Address _Electronic_address 'Keller and Wuthrich' . . stop_ loop_ _Task 'chemical shift assignment' stop_ _Details . save_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-1H_NOESY_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _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_ ####################### # Sample conditions # ####################### save_sample_conditions_1 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 6.5 . pH pressure 1 . atm temperature 285 . 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 DSS H 1 'methyl protons' ppm 0.00 internal direct . . . 1.000000000 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_ _Software_label $CARA stop_ loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-1H TOCSY' 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 L-Dfp6,D-Trp8-SRIF _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 ALA HB H 1.293 0.000 . 2 1 1 ALA H H 7.903 0.000 . 3 1 1 ALA HA H 3.891 0.000 . 4 2 2 GLY H H 8.473 0.000 . 5 2 2 GLY HA2 H 3.747 0.000 . 6 3 3 CYS H H 8.269 0.001 . 7 3 3 CYS HA H 4.379 0.000 . 8 3 3 CYS HB2 H 2.896 0.001 . 9 3 3 CYS HB3 H 2.718 0.000 . 10 4 4 LYS H H 8.427 0.001 . 11 4 4 LYS HA H 4.341 0.001 . 12 4 4 LYS HB2 H 1.407 0.000 . 13 4 4 LYS HB3 H 1.241 0.185 . 14 4 4 LYS HG2 H 1.097 0.002 . 15 4 4 LYS HG3 H 1.001 0.004 . 16 4 4 LYS HD2 H 1.187 0.066 . 17 4 4 LYS HD3 H 1.175 0.004 . 18 4 4 LYS HE2 H 2.541 0.000 . 19 4 4 LYS HZ H 7.206 0.000 . 20 5 5 ASN H H 8.313 0.000 . 21 5 5 ASN HA H 4.577 0.004 . 22 5 5 ASN HB2 H 2.421 0.003 . 23 5 5 ASN HD21 H 6.734 0.002 . 24 5 5 ASN HD22 H 7.327 0.001 . 25 6 6 WFP HA H 4.492 0.001 . 26 6 6 WFP HB2 H 2.718 0.003 . 27 6 6 WFP HB3 H 2.587 0.001 . 28 6 6 WFP HZ H 6.484 0.000 . 29 6 6 WFP HN H 8.283 0.001 . 30 6 6 WFP HD1 H 6.390 0.238 . 31 7 7 PHE H H 8.083 0.002 . 32 7 7 PHE HA H 4.303 0.004 . 33 7 7 PHE HB2 H 2.710 0.002 . 34 7 7 PHE HD1 H 6.973 0.002 . 35 7 7 PHE HD2 H 6.973 0.002 . 36 7 7 PHE HE1 H 7.112 0.001 . 37 7 7 PHE HE2 H 7.112 0.001 . 38 7 7 PHE HZ H 7.057 0.001 . 39 8 8 DTR HA H 4.194 0.002 . 40 8 8 DTR HB2 H 2.806 0.001 . 41 8 8 DTR HB3 H 2.706 0.002 . 42 8 8 DTR HD1 H 6.869 0.002 . 43 8 8 DTR HE1 H 9.316 1.278 . 44 8 8 DTR HE3 H 7.345 0.002 . 45 8 8 DTR HZ2 H 7.237 0.001 . 46 8 8 DTR HZ3 H 6.915 0.002 . 47 8 8 DTR HH2 H 6.995 0.001 . 48 8 8 DTR HN H 8.290 0.002 . 49 9 9 LYS H H 8.078 0.001 . 50 9 9 LYS HA H 3.869 0.001 . 51 9 9 LYS HB2 H 1.322 0.002 . 52 9 9 LYS HB3 H 0.964 0.004 . 53 9 9 LYS HG2 H 0.276 0.009 . 54 9 9 LYS HG3 H 0.100 0.006 . 55 9 9 LYS HD2 H 1.063 0.006 . 56 9 9 LYS HE2 H 2.429 0.008 . 57 9 9 LYS HE3 H 2.355 0.002 . 58 9 9 LYS HZ H 7.227 0.000 . 59 10 10 THR H H 7.699 0.001 . 60 10 10 THR HA H 4.181 0.001 . 61 10 10 THR HB H 3.906 0.001 . 62 10 10 THR HG2 H 0.878 0.003 . 63 11 11 PHE H H 8.258 0.011 . 64 11 11 PHE HA H 4.794 0.001 . 65 11 11 PHE HB2 H 2.667 0.005 . 66 11 11 PHE HB3 H 2.612 0.003 . 67 11 11 PHE HD1 H 6.823 0.143 . 68 11 11 PHE HD2 H 6.823 0.143 . 69 11 11 PHE HE1 H 6.926 0.258 . 70 11 11 PHE HE2 H 6.926 0.258 . 71 11 11 PHE HZ H 6.966 0.002 . 72 12 12 THR H H 8.210 0.001 . 73 12 12 THR HA H 4.244 0.002 . 74 12 12 THR HB H 3.965 0.002 . 75 12 12 THR HG2 H 0.919 0.005 . 76 13 13 SER H H 8.203 0.001 . 77 13 13 SER HA H 4.337 0.002 . 78 13 13 SER HB2 H 3.683 0.003 . 79 14 14 CYS H H 8.001 0.001 . 80 14 14 CYS HA H 4.234 0.001 . 81 14 14 CYS HB2 H 2.978 0.004 . 82 14 14 CYS HB3 H 2.885 0.002 . stop_ save_