data_25739 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Synthesis, Characterization and In Vitro Evaluation of New 99mTc/Re(V)-cyclized Octreotide Analogues: An Experimental and Computational Approach ; _BMRB_accession_number 25739 _BMRB_flat_file_name bmr25739.str _Entry_type original _Submission_date 2015-08-01 _Accession_date 2015-08-01 _Entry_origination author _NMR_STAR_version 2.1.1 _Experimental_method NMR _Details '1H and 13C chemical shifts of ReO-SDPhe-TATE isomer 4' loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Li Yawen . . 2 Ma Lixin . . 3 Gaddam Vikram . . 4 Gallazzi Fabio . . 5 Hennkens Heather M. . 6 Harmata Michael . . 7 Lewis Michael R. . 8 Deakyne Carol A. . 9 Jurisson Silvia S. . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 1 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 52 "13C chemical shifts" 26 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2016-10-28 original BMRB . stop_ loop_ _Related_BMRB_accession_number _Relationship 25506 'Re-SDPhe-TATE isomer 1' 25507 'Linear SDPhe-TATE' 25738 'Re-SDPhe-TATE isomer 2' stop_ _Original_release_date 2016-10-28 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; Synthesis, Characterization, and In Vitro Evaluation of New (99m)Tc/Re(V)-Cyclized Octreotide Analogues: An Experimental and Computational Approach ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 26789775 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Li Yawen . . 2 Ma Lixin . . 3 Gaddam Vikram . . 4 Gallazzi Fabio . . 5 Hennkens Heather M. . 6 Harmata Michael . . 7 Lewis Michael R. . 8 Deakyne Carol A. . 9 Jurisson Silvia S. . stop_ _Journal_abbreviation 'Inorg. Chem.' _Journal_volume 55 _Journal_issue 3 _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 1124 _Page_last 1133 _Year 2016 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Re-SDPhe-TATE isomer 4' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label 'Re-SDPhe-TATE isomer 4' $Re-SDPhe-TATE_isomer_4 Perrhenate $entity_REO stop_ _System_molecular_weight 1268 _System_physical_state native _System_oligomer_state ? _System_paramagnetic no _System_thiol_state . _Database_query_date . _Details . save_ ######################## # Monomeric polymers # ######################## save_Re-SDPhe-TATE_isomer_4 _Saveframe_category monomeric_polymer _Mol_type polymer _Name_common Re-SDPhe-TATE_isomer_4 _Molecular_mass . _Mol_thiol_state 'all other bound' _Details 'ReO is coordinated to the sulfur of SDPhe1, the backbone amide of Cys2, and the sulfurs of Cys2 and Cys7' ############################## # Polymer residue sequence # ############################## _Residue_count 8 _Mol_residue_sequence ; XCYWKTCT ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 SDF-1 2 2 CYS 3 3 TYR 4 4 TRP 5 5 LYS 6 6 THR 7 7 CYS 8 8 THR stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ############# # Ligands # ############# save_REO _Saveframe_category ligand _Mol_type NON-POLYMER _Name_common PERRHENATE _BMRB_code REO _PDB_code REO _Molecular_mass 250.205 _Mol_charge -1 _Mol_paramagnetic . _Mol_aromatic no _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons RE RE RE . 0 . ? O12 O12 O . 0 . ? O13 O13 O . 0 . ? O14 O14 O . 0 . ? O15 O15 O . -1 . ? 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 RE O12 ? ? DOUB RE O13 ? ? DOUB RE O14 ? ? SING RE O15 ? ? stop_ save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species $Re-SDPhe-TATE_isomer_4 . . . . . . 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 $Re-SDPhe-TATE_isomer_4 '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 $Re-SDPhe-TATE_isomer_4 1 mM 'natural abundance' H2O 71 % 'natural abundance' D2O 10 % na CD3CN 19 % na stop_ save_ ############################ # Computer software used # ############################ save_SPARKY _Saveframe_category software _Name SPARKY _Version . loop_ _Vendor _Address _Electronic_address Goddard . . stop_ loop_ _Task 'chemical shift assignment' 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_ ######################### # Experimental detail # ######################### ################################## # NMR Spectrometer definitions # ################################## save_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Varian _Model INOVA _Field_strength 600 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 800 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-13C_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC' _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_ ####################### # 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 . M pH 4 0.5 pH pressure 1 . atm temperature 273 . 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 C 13 'methyl protons' ppm 0.00 na indirect . . . 0.251449530 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_ _Experiment_label '2D 1H-13C HSQC' '2D 1H-1H TOCSY' '2D 1H-1H NOESY' 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 'Re-SDPhe-TATE isomer 4' _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 SDF-1 HA H 4.56 0.01 1 2 1 1 SDF-1 HB2 H 3.04 0.01 2 3 1 1 SDF-1 HB3 H 3.64 0.01 2 4 1 1 SDF-1 HD1 H 7.47 0.01 3 5 1 1 SDF-1 HD2 H 7.47 0.01 3 6 1 1 SDF-1 HE1 H 7.41 0.01 3 7 1 1 SDF-1 HE2 H 7.41 0.01 3 8 1 1 SDF-1 HZ H 7.42 0.01 1 9 1 1 SDF-1 CB C 37.4 0.1 1 10 1 1 SDF-1 CD1 C 124.1 0.1 3 11 1 1 SDF-1 CD2 C 124.1 0.1 3 12 1 1 SDF-1 CE1 C 125.3 0.1 3 13 1 1 SDF-1 CE2 C 125.3 0.1 3 14 1 1 SDF-1 CZ C 122.4 0.1 1 15 2 2 CYS HA H 5.46 0.01 1 16 2 2 CYS HB2 H 3.38 0.01 2 17 2 2 CYS HB3 H 3.55 0.01 2 18 3 3 TYR H H 7.71 0.01 1 19 3 3 TYR HA H 4.45 0.01 1 20 3 3 TYR HB2 H 3.04 0.01 2 21 3 3 TYR HB3 H 3.16 0.01 2 22 3 3 TYR HD1 H 7.24 0.01 3 23 3 3 TYR HD2 H 7.24 0.01 3 24 3 3 TYR HE1 H 7.01 0.01 3 25 3 3 TYR HE2 H 7.01 0.01 3 26 3 3 TYR CA C 51.9 0.1 1 27 3 3 TYR CB C 30.9 0.1 1 28 3 3 TYR CD1 C 126.3 0.1 3 29 3 3 TYR CD2 C 126.3 0.1 3 30 3 3 TYR CE1 C 111.3 0.1 3 31 3 3 TYR CE2 C 111.3 0.1 3 32 4 4 TRP H H 7.86 0.01 1 33 4 4 TRP HA H 4.62 0.01 1 34 4 4 TRP HB2 H 3.14 0.01 2 35 4 4 TRP HB3 H 3.30 0.01 2 36 4 4 TRP HD1 H 7.06 0.01 1 37 4 4 TRP HE1 H 10.19 0.01 1 38 4 4 TRP HE3 H 7.54 0.01 1 39 4 4 TRP HZ2 H 7.66 0.01 1 40 4 4 TRP HZ3 H 7.28 0.01 1 41 4 4 TRP HH2 H 7.37 0.01 1 42 4 4 TRP CB C 21.3 0.1 1 43 4 4 TRP CD1 C 120.2 0.1 1 44 4 4 TRP CE3 C 114.1 0.1 1 45 4 4 TRP CZ2 C 107.5 0.1 1 46 4 4 TRP CZ3 C 115.0 0.1 1 47 4 4 TRP CH2 C 117.5 0.1 1 48 5 5 LYS H H 8.05 0.01 1 49 5 5 LYS HA H 4.18 0.01 1 50 5 5 LYS HB2 H 1.70 0.01 2 51 5 5 LYS HB3 H 1.70 0.01 2 52 5 5 LYS HG2 H 1.04 0.01 2 53 5 5 LYS HG3 H 1.04 0.01 2 54 5 5 LYS HD2 H 1.59 0.01 2 55 5 5 LYS HD3 H 1.59 0.01 2 56 5 5 LYS HE2 H 2.93 0.01 2 57 5 5 LYS HE3 H 2.93 0.01 2 58 5 5 LYS HZ H 7.53 0.01 1 59 5 5 LYS CG C 17.3 0.1 1 60 5 5 LYS CD C 21.7 0.1 1 61 5 5 LYS CE C 34.7 0.1 1 62 6 6 THR H H 7.23 0.01 1 63 6 6 THR HA H 4.26 0.01 1 64 6 6 THR HB H 4.43 0.01 2 65 6 6 THR HG2 H 1.38 0.01 2 66 6 6 THR CA C 55.9 0.1 1 67 6 6 THR CB C 62.2 0.1 1 68 7 7 CYS H H 7.95 0.01 1 69 7 7 CYS HA H 5.37 0.01 1 70 7 7 CYS HB2 H 4.34 0.01 2 71 7 7 CYS HB3 H 4.34 0.01 2 72 7 7 CYS CB C 29.6 0.1 1 73 8 8 THR H H 7.52 0.01 1 74 8 8 THR HA H 4.46 0.01 1 75 8 8 THR HB H 4.43 0.01 2 76 8 8 THR HG2 H 1.31 0.01 2 77 8 8 THR CA C 54.5 0.1 1 78 8 8 THR CB C 63.2 0.1 1 stop_ save_