data_34280 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; Tc-DNA/DNA duplex ; _BMRB_accession_number 34280 _BMRB_flat_file_name bmr34280.str _Entry_type original _Submission_date 2018-06-05 _Accession_date 2018-06-05 _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 Istrate A. . . 2 Johannsen S. . . 3 Istrate A. . . 4 Sigel R. K.O. . 5 Leumann C. . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 234 "13C chemical shifts" 59 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2019-08-06 update BMRB 'update entry citation' 2018-06-07 original author 'original release' stop_ _Original_release_date 2018-06-07 save_ ############################# # Citation for this entry # ############################# save_citation_1 _Saveframe_category entry_citation _Citation_full . _Citation_title ; NMR solution structure of tricyclo-DNA containing duplexes: insight into enhanced thermal stability and nuclease resistance ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 30916334 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Istrate A. . . 2 Johannsen S. . . 3 Istrate A. . . 4 Sigel R. K.O. . 5 Leumann C. . . stop_ _Journal_abbreviation 'Nucleic Acids Res.' _Journal_name_full 'Nucleic acids research' _Journal_volume 47 _Journal_issue 9 _Journal_ISSN 1362-4962 _Journal_CSD 0353 _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 4872 _Page_last 4882 _Year 2019 _Details . save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name 'Tc-DNA/DNA duplex' _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label entity_1 $entity_1 entity_2 $entity_2 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 DNA _Name_common entity_1 _Molecular_mass 3352.575 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 10 _Mol_residue_sequence ; XXXXXXXXAX ; loop_ _Residue_seq_code _Residue_label 1 F7H 2 EAN 3 TCJ 4 F4Q 5 F4Q 6 TCJ 7 EAN 8 EAN 9 TCY 10 TCJ stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ save_entity_2 _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class DNA _Name_common entity_2 _Molecular_mass 3094.042 _Mol_thiol_state 'not present' _Details . _Residue_count 10 _Mol_residue_sequence ; GTAAGCCGAG ; loop_ _Residue_seq_code _Residue_label 1 DG 2 DT 3 DA 4 DA 5 DG 6 DC 7 DC 8 DG 9 DA 10 DG stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . save_ ###################### # Polymer residues # ###################### save_chem_comp_EAN _Saveframe_category polymer_residue _Mol_type 'DNA LINKING' _Name_common ; [(1~{S},2~{R},4~{R},6~{S},8~{R})-8-[5-methyl-2,4-bis(oxidanylidene)pyrimidin-1-yl]-6-oxidanyl-9-oxatricyclo[4.3.0.0^{2,4}]nonan-2-yl] dihydrogen phosphate ; _BMRB_code EAN _PDB_code EAN _Standard_residue_derivative . _Molecular_mass 360.256 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C7 C7 C . 0 . ? C6 C6 C . 0 . ? C5 C5 C . 0 . ? C4 C4 C . 0 . ? C2 C2 C . 0 . ? P P P . 0 . ? O1P O1P O . 0 . ? O2P O2P O . 0 . ? O5' O5' O . 0 . ? C5' C5' C . 0 . ? C4' C4' C . 0 . ? O4' O4' O . 0 . ? C1' C1' C . 0 . ? N1 N1 N . 0 . ? O4 O4 O . 0 . ? N3 N3 N . 0 . ? O2 O2 O . 0 . ? C3' C3' C . 0 . ? C2' C2' C . 0 . ? C7' C7' C . 0 . ? C6' C6' C . 0 . ? C8' C8' C . 0 . ? O3' O3' O . 0 . ? O3P O3P O . 0 . ? H73 H73 H . 0 . ? H71 H71 H . 0 . ? H72 H72 H . 0 . ? H6 H6 H . 0 . ? H1 H1 H . 0 . ? H4' H4' H . 0 . ? H1' H1' H . 0 . ? H3 H3 H . 0 . ? H2' H2' H . 0 . ? H2'' H2'' H . 0 . ? H7' H7' H . 0 . ? H7'' H7'' H . 0 . ? H6' H6' H . 0 . ? H8' H8' H . 0 . ? H8'' H8'' H . 0 . ? H2 H2 H . 0 . ? H4 H4 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 O2 C2 ? ? DOUB O1P P ? ? SING O4' C1' ? ? SING O4' C4' ? ? SING C2 N3 ? ? SING C2 N1 ? ? SING C1' N1 ? ? SING C1' C2' ? ? SING N3 C4 ? ? SING N1 C6 ? ? SING P O5' ? ? SING P O2P ? ? DOUB C4 O4 ? ? SING C4 C5 ? ? DOUB C6 C5 ? ? SING C5 C7 ? ? SING C4' C5' ? ? SING C4' C3' ? ? SING O5' C5' ? ? SING C2' C3' ? ? SING C5' C6' ? ? SING C5' C8' ? ? SING C3' O3' ? ? SING C3' C7' ? ? SING C6' C8' ? ? SING C6' C7' ? ? SING P O3P ? ? SING C7 H73 ? ? SING C7 H71 ? ? SING C7 H72 ? ? SING C6 H6 ? ? SING O2P H1 ? ? SING C4' H4' ? ? SING C1' H1' ? ? SING N3 H3 ? ? SING C2' H2' ? ? SING C2' H2'' ? ? SING C7' H7' ? ? SING C7' H7'' ? ? SING C6' H6' ? ? SING C8' H8' ? ? SING C8' H8'' ? ? SING O3' H2 ? ? SING O3P H4 ? ? stop_ save_ save_chem_comp_F4Q _Saveframe_category polymer_residue _Mol_type 'DNA LINKING' _Name_common ; [(1~{S},2~{R},4~{R},6~{S},8~{R})-8-(2-azanyl-6-oxidanylidene-1~{H}-purin-9-yl)-6-oxidanyl-9-oxatricyclo[4.3.0.0^{2,4}]nonan-2-yl] dihydrogen phosphate ; _BMRB_code F4Q _PDB_code F4Q _Standard_residue_derivative . _Molecular_mass 385.269 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons C8 C8 C . 0 . ? C2 C2 C . 0 . ? C4 C4 C . 0 . ? C5 C5 C . 0 . ? C6 C6 C . 0 . ? P P P . 0 . ? O1P O1P O . 0 . ? O2P O2P O . 0 . ? O5' O5' O . 0 . ? C5' C5' C . 0 . ? C4' C4' C . 0 . ? O4' O4' O . 0 . ? C1' C1' C . 0 . ? N9 N9 N . 0 . ? N7 N7 N . 0 . ? O6 O6 O . 0 . ? N1 N1 N . 0 . ? N2 N2 N . 0 . ? N3 N3 N . 0 . ? C3' C3' C . 0 . ? C2' C2' C . 0 . ? C7' C7' C . 0 . ? C6' C6' C . 0 . ? C8' C8' C . 0 . ? O3' O3' O . 0 . ? H8 H8 H . 0 . ? H3 H3 H . 0 . ? H4' H4' H . 0 . ? H1' H1' H . 0 . ? H1 H1 H . 0 . ? H22 H22 H . 0 . ? H21 H21 H . 0 . ? H2' H2' H . 0 . ? H2'' H2'' H . 0 . ? H7' H7' H . 0 . ? H7'' H7'' H . 0 . ? H6' H6' H . 0 . ? H8' H8' H . 0 . ? H8'' H8'' H . 0 . ? H4 H4 H . 0 . ? OP3 OP3 O . 0 . ? H6 H6 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 O1P P ? ? SING O4' C1' ? ? SING O4' C4' ? ? SING P O2P ? ? SING P O5' ? ? SING C1' N9 ? ? SING C1' C2' ? ? DOUB N3 C2 ? ? SING N3 C4 ? ? SING N2 C2 ? ? SING C2 N1 ? ? SING N9 C4 ? ? SING N9 C8 ? ? DOUB C4 C5 ? ? DOUB C8 N7 ? ? SING N1 C6 ? ? SING C5 C6 ? ? SING C5 N7 ? ? DOUB C6 O6 ? ? SING O5' C5' ? ? SING C4' C5' ? ? SING C4' C3' ? ? SING C2' C3' ? ? SING C5' C6' ? ? SING C5' C8' ? ? SING C3' O3' ? ? SING C3' C7' ? ? SING C6' C8' ? ? SING C6' C7' ? ? SING C8 H8 ? ? SING O2P H3 ? ? SING C4' H4' ? ? SING C1' H1' ? ? SING N1 H1 ? ? SING N2 H22 ? ? SING N2 H21 ? ? SING C2' H2' ? ? SING C2' H2'' ? ? SING C7' H7' ? ? SING C7' H7'' ? ? SING C6' H6' ? ? SING C8' H8' ? ? SING C8' H8'' ? ? SING O3' H4 ? ? SING P OP3 ? ? SING OP3 H6 ? ? stop_ save_ save_chem_comp_F7H _Saveframe_category polymer_residue _Mol_type 'DNA LINKING' _Name_common 4-azanyl-1-[(1~{S},2~{R},4~{S},6~{S},8~{R})-2,6-bis(oxidanyl)-9-oxatricyclo[4.3.0.0^{2,4}]nonan-8-yl]-5-methyl-pyrimidin-2-one _BMRB_code F7H _PDB_code F7H _Standard_residue_derivative . _Molecular_mass 279.292 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons O5' O5' O . 0 . ? C5' C5' C . 0 . ? C4' C4' C . 0 . ? O4' O4' O . 0 . ? C1' C1' C . 0 . ? N1 N1 N . 0 . ? C6 C6 C . 0 . ? C5 C5 C . 0 . ? C7 C7 C . 0 . ? C4 C4 C . 0 . ? N4 N4 N . 0 . ? N3 N3 N . 0 . ? C2 C2 C . 0 . ? O2 O2 O . 0 . ? C3' C3' C . 0 . ? C2' C2' C . 0 . ? C7' C7' C . 0 . ? C6' C6' C . 0 . ? C8' C8' C . 0 . ? O3' O3' O . 0 . ? HO5' HO5' H . 0 . ? H4' H4' H . 0 . ? H1' H1' H . 0 . ? H6 H6 H . 0 . ? H71 H71 H . 0 . ? H72 H72 H . 0 . ? H73 H73 H . 0 . ? H41 H41 H . 0 . ? H42 H42 H . 0 . ? H2' H2' H . 0 . ? H2'' H2'' H . 0 . ? H7' H7' H . 0 . ? H7'' H7'' H . 0 . ? H6' H6' H . 0 . ? H8' H8' H . 0 . ? H8'' H8'' H . 0 . ? H1 H1 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 O4' C1' ? ? SING O4' C4' ? ? SING C1' N1 ? ? SING C1' C2' ? ? SING O5' C5' ? ? DOUB O2 C2 ? ? SING C4' C5' ? ? SING C4' C3' ? ? SING N1 C2 ? ? SING N1 C6 ? ? SING C2 N3 ? ? DOUB C6 C5 ? ? SING C5' C8' ? ? SING C5' C6' ? ? DOUB N3 C4 ? ? SING C2' C3' ? ? SING C5 C4 ? ? SING C5 C7 ? ? SING C4 N4 ? ? SING C3' O3' ? ? SING C3' C7' ? ? SING C8' C6' ? ? SING C6' C7' ? ? SING O5' HO5' ? ? SING C4' H4' ? ? SING C1' H1' ? ? SING C6 H6 ? ? SING C7 H71 ? ? SING C7 H72 ? ? SING C7 H73 ? ? SING N4 H41 ? ? SING N4 H42 ? ? SING C2' H2' ? ? SING C2' H2'' ? ? SING C7' H7' ? ? SING C7' H7'' ? ? SING C6' H6' ? ? SING C8' H8' ? ? SING C8' H8'' ? ? SING O3' H1 ? ? stop_ save_ save_chem_comp_TCJ _Saveframe_category polymer_residue _Mol_type 'DNA LINKING' _Name_common ; [(1~{S},2~{R},4~{R},6~{S},8~{R})-8-(4-azanyl-5-methyl-2-oxidanylidene-pyrimidin-1-yl)-6-oxidanyl-9-oxatricyclo[4.3.0.0^{2,4}]nonan-2-yl] dihydrogen phosphate ; _BMRB_code TCJ _PDB_code TCJ _Standard_residue_derivative . _Molecular_mass 359.272 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons P P P . 0 . ? O1P O1P O . 0 . ? O2P O2P O . 0 . ? O5' O5' O . 0 . ? C5' C5' C . 0 . ? C4' C4' C . 0 . ? O4' O4' O . 0 . ? C1' C1' C . 0 . ? N1 N1 N . 0 . ? C6 C6 C . 0 . ? C5 C5 C . 0 . ? C7 C7 C . 0 . ? C4 C4 C . 0 . ? N4 N4 N . 0 . ? N3 N3 N . 0 . ? C2 C2 C . 0 . ? O2 O2 O . 0 . ? C3' C3' C . 0 . ? C2' C2' C . 0 . ? C7' C7' C . 0 . ? C6' C6' C . 0 . ? C8' C8' C . 0 . ? O3' O3' O . 0 . ? H2 H2 H . 0 . ? H4' H4' H . 0 . ? H1' H1' H . 0 . ? H6 H6 H . 0 . ? H73 H73 H . 0 . ? H71 H71 H . 0 . ? H72 H72 H . 0 . ? H41 H41 H . 0 . ? H42 H42 H . 0 . ? H2' H2' H . 0 . ? H2'' H2'' H . 0 . ? H7' H7' H . 0 . ? H7'' H7'' H . 0 . ? H6' H6' H . 0 . ? H8' H8' H . 0 . ? H8'' H8'' H . 0 . ? H3T H3T H . 0 . ? OP3 OP3 O . 0 . ? H1 H1 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 O2 C2 ? ? SING N3 C2 ? ? DOUB N3 C4 ? ? SING C2 N1 ? ? SING N4 C4 ? ? SING C4 C5 ? ? SING N1 C1' ? ? SING N1 C6 ? ? SING C1' O4' ? ? SING C1' C2' ? ? DOUB C5 C6 ? ? SING C5 C7 ? ? SING O4' C4' ? ? DOUB O1P P ? ? SING C2' C3' ? ? SING P O5' ? ? SING P O2P ? ? SING C4' C3' ? ? SING C4' C5' ? ? SING O5' C5' ? ? SING C3' O3' ? ? SING C3' C7' ? ? SING C5' C6' ? ? SING C5' C8' ? ? SING C7' C6' ? ? SING C6' C8' ? ? SING O2P H2 ? ? SING C4' H4' ? ? SING C1' H1' ? ? SING C6 H6 ? ? SING C7 H73 ? ? SING C7 H71 ? ? SING C7 H72 ? ? SING N4 H41 ? ? SING N4 H42 ? ? SING C2' H2' ? ? SING C2' H2'' ? ? SING C7' H7' ? ? SING C7' H7'' ? ? SING C6' H6' ? ? SING C8' H8' ? ? SING C8' H8'' ? ? SING O3' H3T ? ? SING P OP3 ? ? SING OP3 H1 ? ? stop_ save_ save_chem_comp_TCY _Saveframe_category polymer_residue _Mol_type 'DNA LINKING' _Name_common ; (2R,3aS,4aR,5aR,5bS)-2-(6-amino-9H-purin-9-yl)-3a-hydroxyhexahydrocyclopropa[4,5]cyclopenta[1,2-b]furan-5a(4H)-yl dihydrogen phosphate ; _BMRB_code TCY _PDB_code TCY _Standard_residue_derivative . _Molecular_mass 369.270 _Mol_paramagnetic . _Details . loop_ _Atom_name _PDB_atom_name _Atom_type _Atom_chirality _Atom_charge _Atom_oxidation_number _Atom_unpaired_electrons O3P O3P O . 0 . ? O1P O1P O . 0 . ? P P P . 0 . ? O2P O2P O . 0 . ? C8' C8' C . 0 . ? O5' O5' O . 0 . ? C5' C5' C . 0 . ? C6' C6' C . 0 . ? C4' C4' C . 0 . ? C3' C3' C . 0 . ? C7' C7' C . 0 . ? O3' O3' O . 0 . ? C2' C2' C . 0 . ? C1' C1' C . 0 . ? O4' O4' O . 0 . ? N9 N9 N . 0 . ? C4 C4 C . 0 . ? N3 N3 N . 0 . ? C2 C2 C . 0 . ? N1 N1 N . 0 . ? C6 C6 C . 0 . ? N6 N6 N . 0 . ? C5 C5 C . 0 . ? N7 N7 N . 0 . ? C8 C8 C . 0 . ? H8' H8' H . 0 . ? H8'A H8'A H . 0 . ? H6' H6' H . 0 . ? H4' H4' H . 0 . ? H7' H7' H . 0 . ? H7'A H7'A H . 0 . ? HO3' HO3' H . 0 . ? H2' H2' H . 0 . ? H2'A H2'A H . 0 . ? H1' H1' H . 0 . ? H2 H2 H . 0 . ? HN6 HN6 H . 0 . ? HN6A HN6A H . 0 . ? H8 H8 H . 0 . ? HO3P HO3P H . 0 . ? HO2P HO2P 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 O3P P ? ? DOUB O1P P ? ? SING P O2P ? ? SING P O5' ? ? SING C8' C5' ? ? SING C8' C6' ? ? SING O5' C5' ? ? SING C5' C6' ? ? SING C5' C4' ? ? SING C6' C7' ? ? SING C4' C3' ? ? SING C4' O4' ? ? SING C3' C7' ? ? SING C3' O3' ? ? SING C3' C2' ? ? SING C2' C1' ? ? SING C1' O4' ? ? SING C1' N9 ? ? SING N9 C4 ? ? SING N9 C8 ? ? DOUB C4 N3 ? ? SING C4 C5 ? ? SING N3 C2 ? ? DOUB C2 N1 ? ? SING N1 C6 ? ? SING C6 N6 ? ? DOUB C6 C5 ? ? SING C5 N7 ? ? DOUB N7 C8 ? ? SING C8' H8' ? ? SING C8' H8'A ? ? SING C6' H6' ? ? SING C4' H4' ? ? SING C7' H7' ? ? SING C7' H7'A ? ? SING O3' HO3' ? ? SING C2' H2' ? ? SING C2' H2'A ? ? SING C1' H1' ? ? SING C2 H2 ? ? SING N6 HN6 ? ? SING N6 HN6A ? ? SING C8 H8 ? ? SING O3P HO3P ? ? SING O2P HO2P ? ? 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 Human 9606 Eukaryota Metazoa Homo sapiens $entity_2 Human 9606 Eukaryota Metazoa Homo sapiens 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' . . . . . $entity_2 'chemical synthesis' . . . . . stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_sample_1 _Saveframe_category sample _Sample_type solution _Details '0.5 mM tc-DNA/DNA, 50 mM NaCl, 10 mM NaH2PO4, 100% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 0.5 mM 'natural abundance' $entity_2 0.5 mM 'natural abundance' NaCl 50 mM 'natural abundance' NaH2PO4 10 mM 'natural abundance' stop_ save_ save_sample_2 _Saveframe_category sample _Sample_type solution _Details '0.5 mM tc-DNA/DNA, 50 mM NaCl, 10 mM NaH2PO4, 90% H2O/10% D2O' loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $entity_1 0.5 mM 'natural abundance' $entity_2 0.5 mM 'natural abundance' NaCl 50 mM 'natural abundance' NaH2PO4 10 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_software_1 _Saveframe_category software _Name CNS _Version . loop_ _Vendor _Address _Electronic_address 'Brunger, Adams, Clore, Gros, Nilges and Read' . . stop_ loop_ _Task refinement stop_ _Details . save_ save_software_2 _Saveframe_category software _Name GROMOS _Version . loop_ _Vendor _Address _Electronic_address 'van Gunsteren and Berendsen' . . stop_ loop_ _Task refinement 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 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_NMR_spectrometer_1 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model AvanceII _Field_strength 700 _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_NOESY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _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_2 save_ save_2D_1H-1H_TOCSY_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _Sample_label $sample_1 save_ save_2D_DQF-COSY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $sample_1 save_ save_2D_1H-13C_HSQC_6 _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 7.05 . pH pressure 1 . atm temperature 298 . K stop_ save_ save_sample_conditions_2 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 7.05 . pH pressure 1 . atm temperature 283 . K stop_ save_ save_sample_conditions_3 _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units pH 7.05 . pH pressure 1 . atm temperature 283 . 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_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-1H TOCSY' '2D DQF-COSY' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_1 $sample_2 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 F7H H1' H 6.187 0.002 1 2 1 1 F7H H2' H 2.882 0.002 1 3 1 1 F7H H2'' H 3.301 0.002 1 4 1 1 F7H H4' H 4.734 0.003 1 5 1 1 F7H H6 H 7.933 0.001 1 6 1 1 F7H H6' H 1.928 0.003 1 7 1 1 F7H H7' H 2.278 0.002 1 8 1 1 F7H H7'' H 2.453 0.002 1 9 1 1 F7H H8' H 1.106 0.001 1 10 1 1 F7H H8'' H 1.818 0.001 1 11 1 1 F7H H71 H 2.127 0.002 1 12 1 1 F7H H72 H 2.127 0.002 1 13 1 1 F7H H73 H 2.127 0.002 1 14 1 1 F7H C1' C 89.614 0.000 1 15 1 1 F7H C2' C 45.754 0.003 1 16 1 1 F7H C4' C 92.956 0.000 1 17 1 1 F7H C6' C 25.800 0.000 1 18 1 1 F7H C7 C 14.971 0.000 1 19 1 1 F7H C7' C 42.525 0.006 1 20 1 1 F7H C8' C 18.974 0.051 1 21 2 2 EAN H1' H 6.062 0.001 1 22 2 2 EAN H2' H 2.878 0.003 1 23 2 2 EAN H2'' H 3.292 0.005 1 24 2 2 EAN H3 H 14.042 0.001 1 25 2 2 EAN H4' H 4.870 0.001 1 26 2 2 EAN H6 H 7.688 0.001 1 27 2 2 EAN H6' H 2.013 0.006 1 28 2 2 EAN H7' H 2.000 0.001 1 29 2 2 EAN H7'' H 2.751 0.002 1 30 2 2 EAN H8' H 1.334 0.002 1 31 2 2 EAN H8'' H 1.778 0.003 1 32 2 2 EAN H71 H 1.824 0.001 1 33 2 2 EAN H72 H 1.824 0.001 1 34 2 2 EAN H73 H 1.824 0.001 1 35 2 2 EAN C1' C 91.882 0.000 1 36 3 3 TCJ H1' H 6.083 0.001 1 37 3 3 TCJ H2' H 3.184 0.000 1 38 3 3 TCJ H2'' H 3.220 0.005 1 39 3 3 TCJ H4' H 4.914 0.002 1 40 3 3 TCJ H6 H 7.615 0.001 1 41 3 3 TCJ H6' H 2.017 0.003 1 42 3 3 TCJ H7' H 2.102 0.003 1 43 3 3 TCJ H7'' H 2.634 0.002 1 44 3 3 TCJ H8' H 1.325 0.002 1 45 3 3 TCJ H8'' H 1.782 0.002 1 46 3 3 TCJ H41 H 8.991 0.003 1 47 3 3 TCJ H42 H 6.737 0.001 1 48 3 3 TCJ H71 H 1.922 0.002 1 49 3 3 TCJ H72 H 1.922 0.002 1 50 3 3 TCJ H73 H 1.922 0.002 1 51 3 3 TCJ C1' C 91.853 0.000 1 52 3 3 TCJ C4' C 93.413 0.000 1 53 3 3 TCJ C7' C 40.833 0.009 1 54 4 4 F4Q H1 H 13.044 0.002 1 55 4 4 F4Q H1' H 6.158 0.002 1 56 4 4 F4Q H2' H 3.209 0.003 1 57 4 4 F4Q H2'' H 3.285 0.003 1 58 4 4 F4Q H4' H 4.881 0.001 1 59 4 4 F4Q H6' H 1.920 0.002 1 60 4 4 F4Q H7' H 1.722 0.002 1 61 4 4 F4Q H7'' H 2.538 0.001 1 62 4 4 F4Q H8 H 7.709 0.001 1 63 4 4 F4Q H8' H 1.222 0.001 1 64 4 4 F4Q H8'' H 1.777 0.004 1 65 4 4 F4Q C1' C 90.521 0.000 1 66 4 4 F4Q C7' C 41.312 0.012 1 67 5 5 F4Q H1 H 13.098 0.001 1 68 5 5 F4Q H1' H 6.236 0.002 1 69 5 5 F4Q H2' H 3.140 0.002 1 70 5 5 F4Q H2'' H 3.273 0.003 1 71 5 5 F4Q H4' H 4.858 0.002 1 72 5 5 F4Q H6' H 1.923 0.002 1 73 5 5 F4Q H7' H 1.538 0.002 1 74 5 5 F4Q H7'' H 2.674 0.002 1 75 5 5 F4Q H8 H 7.381 0.001 1 76 5 5 F4Q H8' H 1.223 0.002 1 77 5 5 F4Q H8'' H 1.776 0.004 1 78 5 5 F4Q C1' C 90.672 0.000 1 79 6 6 TCJ H1' H 5.935 0.002 1 80 6 6 TCJ H2' H 3.122 0.002 1 81 6 6 TCJ H2'' H 3.211 0.003 1 82 6 6 TCJ H4' H 4.825 0.001 1 83 6 6 TCJ H6 H 7.297 0.001 1 84 6 6 TCJ H6' H 1.897 0.003 1 85 6 6 TCJ H7' H 1.800 0.005 1 86 6 6 TCJ H7'' H 2.677 0.002 1 87 6 6 TCJ H8' H 1.288 0.002 1 88 6 6 TCJ H8'' H 1.772 0.002 1 89 6 6 TCJ H41 H 8.718 0.004 1 90 6 6 TCJ H42 H 6.728 0.002 1 91 6 6 TCJ H71 H 1.594 0.002 1 92 6 6 TCJ H72 H 1.594 0.002 1 93 6 6 TCJ H73 H 1.594 0.002 1 94 6 6 TCJ C1' C 91.999 0.000 1 95 6 6 TCJ C4' C 92.906 0.000 1 96 6 6 TCJ C6' C 24.883 0.000 1 97 7 7 EAN H1' H 6.014 0.002 1 98 7 7 EAN H2' H 3.125 0.001 1 99 7 7 EAN H2'' H 3.296 0.002 1 100 7 7 EAN H3 H 14.404 0.001 1 101 7 7 EAN H4' H 4.852 0.003 1 102 7 7 EAN H6 H 7.592 0.001 1 103 7 7 EAN H6' H 1.998 0.002 1 104 7 7 EAN H7' H 1.946 0.002 1 105 7 7 EAN H7'' H 2.763 0.003 1 106 7 7 EAN H8' H 1.332 0.002 1 107 7 7 EAN H71 H 1.740 0.002 1 108 7 7 EAN H72 H 1.740 0.002 1 109 7 7 EAN H73 H 1.740 0.002 1 110 7 7 EAN C1' C 92.001 0.000 1 111 8 8 EAN H1' H 6.129 0.001 1 112 8 8 EAN H2' H 3.125 0.003 1 113 8 8 EAN H2'' H 3.337 0.002 1 114 8 8 EAN H3 H 13.879 0.007 1 115 8 8 EAN H4' H 4.941 0.001 1 116 8 8 EAN H6 H 7.736 0.001 1 117 8 8 EAN H6' H 2.055 0.002 1 118 8 8 EAN H7' H 2.156 0.002 1 119 8 8 EAN H7'' H 2.756 0.001 1 120 8 8 EAN H8' H 1.343 0.004 1 121 8 8 EAN H8'' H 1.823 0.003 1 122 8 8 EAN H71 H 1.925 0.003 1 123 8 8 EAN H72 H 1.925 0.003 1 124 8 8 EAN H73 H 1.925 0.003 1 125 8 8 EAN C1' C 91.764 0.000 1 126 9 9 TCY H1' H 6.571 0.002 1 127 9 9 TCY H2 H 7.386 0.001 1 128 9 9 TCY H2' H 3.269 0.002 1 129 9 9 TCY H2'A H 3.460 0.002 1 130 9 9 TCY H6' H 1.991 0.002 1 131 9 9 TCY H7' H 1.706 0.003 1 132 9 9 TCY H7'A H 2.744 0.003 1 133 9 9 TCY H8 H 8.162 0.000 1 134 9 9 TCY H8' H 1.309 0.001 1 135 9 9 TCY H8'A H 1.844 0.002 1 136 9 9 TCY C1' C 90.987 0.000 1 137 9 9 TCY HN6 H 8.477 0.006 1 138 9 9 TCY HN6A H 6.620 0.003 1 139 10 10 TCJ H1' H 5.876 0.002 1 140 10 10 TCJ H2' H 2.401 0.002 1 141 10 10 TCJ H2'' H 2.768 0.003 1 142 10 10 TCJ H4' H 4.720 0.001 1 143 10 10 TCJ H6 H 7.260 0.001 1 144 10 10 TCJ H6' H 1.836 0.003 1 145 10 10 TCJ H7' H 1.702 0.000 1 146 10 10 TCJ H7'' H 1.967 0.002 1 147 10 10 TCJ H8' H 1.156 0.002 1 148 10 10 TCJ H8'' H 1.697 0.002 1 149 10 10 TCJ H41 H 8.815 0.002 1 150 10 10 TCJ H42 H 6.943 0.001 1 151 10 10 TCJ H71 H 1.648 0.002 1 152 10 10 TCJ H72 H 1.648 0.002 1 153 10 10 TCJ H73 H 1.648 0.002 1 154 10 10 TCJ C1' C 90.798 0.000 1 155 10 10 TCJ C2' C 49.880 0.025 1 156 10 10 TCJ C4' C 91.973 0.000 1 157 10 10 TCJ C6' C 25.442 0.000 1 158 10 10 TCJ C8' C 17.153 0.000 1 stop_ save_ save_assigned_chemical_shifts_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-1H NOESY' '2D 1H-1H TOCSY' '2D DQF-COSY' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_1 $sample_2 stop_ _Sample_conditions_label $sample_conditions_1 _Chem_shift_reference_set_label $chem_shift_reference_1 _Mol_system_component_name entity_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 11 1 DG H1 H 13.652 0.001 1 2 11 1 DG H1' H 6.287 0.002 1 3 11 1 DG H2' H 3.025 0.003 1 4 11 1 DG H2'' H 3.104 0.003 1 5 11 1 DG H4' H 4.473 0.001 1 6 11 1 DG H5' H 4.162 0.002 1 7 11 1 DG H5'' H 4.063 0.003 1 8 11 1 DG H8 H 8.228 0.001 1 9 11 1 DG C1' C 87.527 0.000 1 10 11 1 DG C4' C 88.324 0.000 1 11 11 1 DG C5' C 63.151 0.006 1 12 12 2 DT H1' H 6.387 0.002 1 13 12 2 DT H2' H 2.607 0.001 1 14 12 2 DT H2'' H 3.008 0.003 1 15 12 2 DT H3 H 13.861 0.000 1 16 12 2 DT H3' H 5.208 0.002 1 17 12 2 DT H4' H 4.629 0.001 1 18 12 2 DT H5' H 4.415 0.003 2 19 12 2 DT H5'' H 4.416 0.000 2 20 12 2 DT H6 H 7.821 0.001 1 21 12 2 DT H71 H 1.509 0.002 1 22 12 2 DT H72 H 1.509 0.002 1 23 12 2 DT H73 H 1.509 0.002 1 24 12 2 DT C1' C 86.271 0.000 1 25 12 2 DT C3' C 79.717 0.000 1 26 12 2 DT C4' C 87.007 0.000 1 27 13 3 DA H1' H 6.369 0.002 1 28 13 3 DA H2 H 6.749 0.001 1 29 13 3 DA H2' H 2.970 0.002 1 30 13 3 DA H2'' H 3.225 0.002 1 31 13 3 DA H3' H 5.322 0.002 1 32 13 3 DA H4' H 4.677 0.001 1 33 13 3 DA H5' H 4.380 0.002 1 34 13 3 DA H5'' H 4.516 0.003 1 35 13 3 DA H8 H 8.451 0.002 1 36 13 3 DA H61 H 8.135 0.000 1 37 13 3 DA H62 H 6.489 0.000 1 38 13 3 DA C1' C 84.803 0.000 1 39 13 3 DA C3' C 79.389 0.000 1 40 13 3 DA C4' C 87.087 0.000 1 41 14 4 DA H1' H 6.239 0.002 1 42 14 4 DA H2 H 7.476 0.000 1 43 14 4 DA H2' H 2.907 0.002 1 44 14 4 DA H2'' H 3.025 0.003 1 45 14 4 DA H3' H 5.294 0.002 1 46 14 4 DA H4' H 4.691 0.002 1 47 14 4 DA H5' H 4.510 0.003 2 48 14 4 DA H5'' H 4.510 0.001 2 49 14 4 DA H8 H 8.197 0.003 1 50 14 4 DA H61 H 8.023 0.000 1 51 14 4 DA H62 H 6.439 0.000 1 52 14 4 DA C1' C 84.233 0.000 1 53 14 4 DA C3' C 78.092 0.000 1 54 14 4 DA C4' C 86.882 0.000 1 55 14 4 DA C5' C 68.087 0.000 1 56 15 5 DG H1 H 13.266 0.001 1 57 15 5 DG H1' H 6.127 0.001 1 58 15 5 DG H2' H 2.749 0.002 1 59 15 5 DG H2'' H 2.915 0.002 1 60 15 5 DG H3' H 5.135 0.002 1 61 15 5 DG H4' H 4.634 0.001 1 62 15 5 DG H5' H 4.469 0.001 2 63 15 5 DG H5'' H 4.469 0.001 3 64 15 5 DG H8 H 7.779 0.001 1 65 15 5 DG C1' C 84.846 0.000 1 66 15 5 DG C3' C 77.925 0.000 1 67 15 5 DG C5' C 68.086 0.000 1 68 16 6 DC H1' H 6.192 0.002 1 69 16 6 DC H2' H 2.442 0.004 1 70 16 6 DC H2'' H 2.757 0.003 1 71 16 6 DC H3' H 5.314 0.000 1 72 16 6 DC H4' H 4.447 0.003 1 73 16 6 DC H5 H 5.278 0.002 1 74 16 6 DC H5' H 4.476 0.004 1 75 16 6 DC H5'' H 4.381 0.003 1 76 16 6 DC H6 H 7.528 0.001 1 77 16 6 DC H41 H 8.229 0.006 1 78 16 6 DC H42 H 6.635 0.004 1 79 16 6 DC C1' C 86.668 0.000 1 80 16 6 DC C4' C 85.448 0.000 1 81 16 6 DC C5 C 97.328 0.000 1 82 16 6 DC C5' C 66.935 0.002 1 83 17 7 DC H1' H 6.149 0.003 1 84 17 7 DC H2' H 2.470 0.004 1 85 17 7 DC H2'' H 2.776 0.002 1 86 17 7 DC H3' H 5.072 0.002 1 87 17 7 DC H4' H 4.418 0.002 1 88 17 7 DC H5 H 5.634 0.002 1 89 17 7 DC H5' H 4.364 0.001 2 90 17 7 DC H5'' H 4.364 0.002 2 91 17 7 DC H6 H 7.679 0.003 1 92 17 7 DC H41 H 8.578 0.003 1 93 17 7 DC H42 H 6.947 0.000 1 94 17 7 DC C1' C 86.644 0.000 1 95 17 7 DC C3' C 77.086 0.000 1 96 17 7 DC C5 C 98.273 0.000 1 97 17 7 DC C5' C 67.158 0.000 1 98 18 8 DG H1 H 12.630 0.001 1 99 18 8 DG H1' H 6.038 0.002 1 100 18 8 DG H2' H 2.788 0.002 1 101 18 8 DG H2'' H 3.044 0.004 1 102 18 8 DG H3' H 5.206 0.001 1 103 18 8 DG H4' H 4.588 0.002 1 104 18 8 DG H5' H 4.322 0.003 1 105 18 8 DG H5'' H 4.404 0.003 1 106 18 8 DG H8 H 7.950 0.001 1 107 18 8 DG C1' C 84.681 0.000 1 108 18 8 DG C3' C 79.971 0.000 1 109 18 8 DG C4' C 87.098 0.000 1 110 18 8 DG C5' C 68.380 0.016 1 111 19 9 DA H1' H 6.295 0.002 1 112 19 9 DA H2 H 7.840 0.000 1 113 19 9 DA H2' H 2.802 0.002 1 114 19 9 DA H2'' H 3.049 0.002 1 115 19 9 DA H3' H 5.258 0.002 1 116 19 9 DA H4' H 4.635 0.003 1 117 19 9 DA H5' H 4.420 0.002 1 118 19 9 DA H5'' H 4.460 0.008 1 119 19 9 DA H8 H 8.229 0.001 1 120 19 9 DA H61 H 8.207 0.010 1 121 19 9 DA H62 H 6.345 0.003 1 122 19 9 DA C1' C 84.778 0.000 1 123 19 9 DA C3' C 78.642 0.000 1 124 19 9 DA C4' C 86.653 0.000 1 125 20 10 DG H1' H 6.293 0.002 1 126 20 10 DG H2' H 2.657 0.003 1 127 20 10 DG H2'' H 2.483 0.003 1 128 20 10 DG H3' H 4.855 0.001 1 129 20 10 DG H4' H 4.413 0.002 1 130 20 10 DG H5' H 4.351 0.003 1 131 20 10 DG H5'' H 4.429 0.004 1 132 20 10 DG H8 H 7.902 0.001 1 133 20 10 DG C1' C 84.438 0.000 1 134 20 10 DG C3' C 72.930 0.000 1 135 20 10 DG C4' C 87.685 0.000 1 stop_ save_