data_34277 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; tc-DNA/tc-DNA duplex ; _BMRB_accession_number 34277 _BMRB_flat_file_name bmr34277.str _Entry_type original _Submission_date 2018-05-29 _Accession_date 2018-05-29 _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" 190 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2019-08-06 update BMRB 'update entry citation' 2018-06-04 original author 'original release' stop_ _Original_release_date 2018-06-01 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/tc-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 3432.555 _Mol_thiol_state 'not present' _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 10 _Mol_residue_sequence ; XXXXXXXXXX ; loop_ _Residue_seq_code _Residue_label 1 TCJ 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 3502.577 _Mol_thiol_state 'not present' _Details . _Residue_count 10 _Mol_residue_sequence ; XXXXXXXXXX ; loop_ _Residue_seq_code _Residue_label 1 F4Q 2 EAN 3 TCY 4 TCY 5 F4Q 6 TCJ 7 TCJ 8 F4Q 9 TCY 10 F4Q 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_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/tc-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/tc-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_ save_sample_3 _Saveframe_category sample _Sample_type solution _Details '0.5 mM tc-DNA/tc-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_ ############################ # 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_DQF-COSY_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D DQF-COSY' _Sample_label $sample_1 save_ save_2D_1H-1H_TOCSY_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H TOCSY' _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_ save_2D_1H-1H_NOESY_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_2 save_ save_2D_1H-1H_NOESY_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $sample_3 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' 60 . mM 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 'ionic strength' 60 . mM 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 'ionic strength' 60 . mM 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 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 DQF-COSY' '2D 1H-1H TOCSY' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_1 $sample_2 $sample_3 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 TCJ H1' H 6.250 0.001 1 2 1 1 TCJ H2' H 3.005 0.001 1 3 1 1 TCJ H2'' H 3.343 0.001 1 4 1 1 TCJ H4' H 4.848 0.001 1 5 1 1 TCJ H6 H 8.124 0.000 1 6 1 1 TCJ H6' H 1.947 0.000 1 7 1 1 TCJ H7' H 2.148 0.002 1 8 1 1 TCJ H7'' H 2.564 0.001 1 9 1 1 TCJ H8' H 1.202 0.000 1 10 1 1 TCJ H8'' H 1.847 0.001 1 11 2 2 EAN H1' H 6.169 0.002 1 12 2 2 EAN H2' H 3.383 0.000 1 13 2 2 EAN H2'' H 3.347 0.002 1 14 2 2 EAN H6 H 7.759 0.033 1 15 2 2 EAN H7' H 2.026 0.004 1 16 2 2 EAN H7'' H 2.771 0.001 1 17 2 2 EAN H71 H 1.849 0.000 1 18 2 2 EAN H72 H 1.849 0.000 1 19 2 2 EAN H73 H 1.849 0.000 1 20 3 3 TCJ H1' H 6.015 0.002 1 21 3 3 TCJ H2' H 3.118 0.000 1 22 3 3 TCJ H2'' H 3.285 0.001 1 23 3 3 TCJ H6 H 7.648 0.003 1 24 3 3 TCJ H7' H 2.069 0.004 1 25 3 3 TCJ H7'' H 2.652 0.003 1 26 3 3 TCJ H41 H 8.901 0.002 1 27 3 3 TCJ H42 H 6.744 0.007 1 28 3 3 TCJ H71 H 1.937 0.001 1 29 3 3 TCJ H72 H 1.937 0.001 1 30 3 3 TCJ H73 H 1.937 0.001 1 31 4 4 F4Q H1 H 12.887 0.001 1 32 4 4 F4Q H1' H 6.214 0.001 1 33 4 4 F4Q H2' H 3.273 0.002 1 34 4 4 F4Q H2'' H 3.345 0.000 1 35 4 4 F4Q H7' H 1.617 0.002 1 36 4 4 F4Q H7'' H 2.557 0.001 1 37 4 4 F4Q H8 H 7.735 0.001 1 38 5 5 F4Q H1 H 13.274 0.002 1 39 5 5 F4Q H1' H 6.380 0.001 1 40 5 5 F4Q H2' H 3.308 0.001 1 41 5 5 F4Q H2'' H 3.344 0.001 1 42 5 5 F4Q H7' H 1.564 0.001 1 43 5 5 F4Q H7'' H 2.733 0.002 1 44 5 5 F4Q H8 H 7.452 0.001 1 45 6 6 TCJ H1' H 6.055 0.001 1 46 6 6 TCJ H2' H 3.047 0.001 1 47 6 6 TCJ H2'' H 3.304 0.001 1 48 6 6 TCJ H4' H 4.856 0.001 1 49 6 6 TCJ H6 H 7.347 0.001 1 50 6 6 TCJ H7' H 1.900 0.001 1 51 6 6 TCJ H7'' H 2.740 0.000 1 52 6 6 TCJ H41 H 8.904 0.001 1 53 6 6 TCJ H42 H 6.767 0.000 1 54 6 6 TCJ H71 H 1.572 0.002 1 55 6 6 TCJ H72 H 1.572 0.002 1 56 6 6 TCJ H73 H 1.572 0.002 1 57 7 7 EAN H1' H 6.098 0.001 1 58 7 7 EAN H2' H 3.152 0.003 1 59 7 7 EAN H2'' H 3.364 0.003 1 60 7 7 EAN H3 H 14.404 0.001 1 61 7 7 EAN H4' H 4.876 0.001 1 62 7 7 EAN H6 H 7.641 0.001 1 63 7 7 EAN H7' H 1.984 0.000 1 64 7 7 EAN H7'' H 2.814 0.004 1 65 7 7 EAN H8' H 1.349 0.001 1 66 7 7 EAN H8'' H 2.012 0.000 1 67 7 7 EAN H71 H 1.732 0.000 1 68 7 7 EAN H72 H 1.732 0.000 1 69 7 7 EAN H73 H 1.732 0.000 1 70 8 8 EAN H1' H 6.020 0.001 1 71 8 8 EAN H2' H 2.925 0.001 1 72 8 8 EAN H2'' H 3.374 0.001 1 73 8 8 EAN H3 H 13.577 0.002 1 74 8 8 EAN H6 H 7.723 0.001 1 75 8 8 EAN H7' H 2.124 0.001 1 76 8 8 EAN H7'' H 2.740 0.001 1 77 8 8 EAN H71 H 1.893 0.003 1 78 8 8 EAN H72 H 1.893 0.003 1 79 8 8 EAN H73 H 1.893 0.003 1 80 9 9 TCY H1' H 6.572 0.001 1 81 9 9 TCY H2 H 7.372 0.001 1 82 9 9 TCY H2' H 3.285 0.003 1 83 9 9 TCY H2'A H 3.461 0.001 1 84 9 9 TCY H7' H 1.607 0.000 1 85 9 9 TCY H7'A H 2.734 0.002 1 86 9 9 TCY H8 H 8.174 0.000 1 87 10 10 TCJ H1' H 5.923 0.001 1 88 10 10 TCJ H2' H 2.443 0.001 1 89 10 10 TCJ H2'' H 2.802 0.003 1 90 10 10 TCJ H4' H 4.724 0.001 1 91 10 10 TCJ H6 H 7.219 0.001 1 92 10 10 TCJ H7' H 2.442 0.001 1 93 10 10 TCJ H7'' H 2.797 0.000 1 94 10 10 TCJ H71 H 1.506 0.000 1 95 10 10 TCJ H72 H 1.506 0.000 1 96 10 10 TCJ H73 H 1.506 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 DQF-COSY' '2D 1H-1H TOCSY' '2D 1H-13C HSQC' stop_ loop_ _Sample_label $sample_1 $sample_2 $sample_3 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 F4Q H1' H 6.465 0.001 1 2 11 1 F4Q H2' H 3.305 0.001 1 3 11 1 F4Q H2'' H 3.414 0.001 1 4 11 1 F4Q H4' H 4.927 0.000 1 5 11 1 F4Q 6H' H 1.906 0.000 1 6 11 1 F4Q H6' H 1.906 0.001 1 7 11 1 F4Q H7' H 1.754 0.003 1 8 11 1 F4Q H7'' H 2.530 0.002 1 9 11 1 F4Q H8 H 8.366 0.001 1 10 11 1 F4Q H8' H 1.158 0.002 1 11 11 1 F4Q H8'' H 1.684 0.002 1 12 12 2 EAN H1' H 6.202 0.001 1 13 12 2 EAN H2' H 3.497 0.001 1 14 12 2 EAN H2'' H 3.412 0.001 1 15 12 2 EAN H3 H 13.422 0.004 1 16 12 2 EAN H6 H 7.597 0.001 1 17 12 2 EAN H7' H 2.152 0.001 1 18 12 2 EAN H7'' H 2.695 0.001 1 19 12 2 EAN H71 H 1.687 0.000 1 20 12 2 EAN H72 H 1.687 0.000 1 21 12 2 EAN H73 H 1.687 0.000 1 22 13 3 TCY H1' H 6.535 0.001 1 23 13 3 TCY H2 H 6.286 0.000 1 24 13 3 TCY H2' H 3.382 0.001 1 25 13 3 TCY H2'A H 3.568 0.002 1 26 13 3 TCY H7' H 1.759 0.003 1 27 13 3 TCY H7'A H 2.656 0.001 1 28 13 3 TCY H8 H 8.323 0.000 1 29 14 4 TCY H1' H 6.472 0.003 1 30 14 4 TCY H2 H 7.401 0.001 1 31 14 4 TCY H2' H 3.408 0.001 1 32 14 4 TCY H2'A H 3.471 0.004 1 33 14 4 TCY H7' H 1.665 0.000 1 34 14 4 TCY H7'A H 2.569 0.004 1 35 14 4 TCY H8 H 7.874 0.001 1 36 15 5 F4Q H1 H 13.435 0.005 1 37 15 5 F4Q H1' H 6.339 0.001 1 38 15 5 F4Q H2' H 3.292 0.001 1 39 15 5 F4Q H2'' H 3.351 0.000 1 40 15 5 F4Q H7' H 1.607 0.000 1 41 15 5 F4Q H7'' H 2.772 0.001 1 42 15 5 F4Q H8 H 7.385 0.001 1 43 16 6 TCJ H1' H 6.050 0.002 1 44 16 6 TCJ H2' H 2.961 0.000 1 45 16 6 TCJ H2'' H 3.299 0.001 1 46 16 6 TCJ H4' H 4.854 0.002 1 47 16 6 TCJ H6 H 7.312 0.001 1 48 16 6 TCJ H7' H 1.935 0.003 1 49 16 6 TCJ H7'' H 2.745 0.004 1 50 16 6 TCJ H41 H 8.893 0.000 1 51 16 6 TCJ H42 H 6.753 0.000 1 52 16 6 TCJ H71 H 1.513 0.001 1 53 16 6 TCJ H72 H 1.513 0.001 1 54 16 6 TCJ H73 H 1.513 0.001 1 55 17 7 TCJ H1' H 5.993 0.001 1 56 17 7 TCJ H2' H 3.136 0.001 1 57 17 7 TCJ H2'' H 3.299 0.001 1 58 17 7 TCJ H4' H 4.864 0.000 1 59 17 7 TCJ H6 H 7.579 0.001 1 60 17 7 TCJ H7' H 2.083 0.001 1 61 17 7 TCJ H7'' H 2.645 0.002 1 62 17 7 TCJ H41 H 8.891 0.000 1 63 17 7 TCJ H42 H 6.684 0.003 1 64 17 7 TCJ H71 H 1.751 0.001 1 65 17 7 TCJ H72 H 1.751 0.001 1 66 17 7 TCJ H73 H 1.751 0.001 1 67 18 8 F4Q H1 H 12.552 0.003 1 68 18 8 F4Q H1' H 6.288 0.001 1 69 18 8 F4Q H2' H 3.231 0.001 1 70 18 8 F4Q H2'' H 3.418 0.001 1 71 18 8 F4Q H7' H 1.759 0.001 1 72 18 8 F4Q H7'' H 2.640 0.003 1 73 18 8 F4Q H8 H 7.837 0.000 1 74 18 8 F4Q H21 H 7.635 0.000 1 75 19 9 TCY H1' H 6.603 0.001 1 76 19 9 TCY H2 H 7.563 0.000 1 77 19 9 TCY H2' H 3.425 0.000 1 78 19 9 TCY H2'A H 3.501 0.002 1 79 19 9 TCY H6' H 1.860 0.003 1 80 19 9 TCY H7' H 1.771 0.000 1 81 19 9 TCY H7'A H 2.560 0.002 1 82 19 9 TCY H8 H 8.039 0.000 1 83 19 9 TCY H8' H 1.245 0.000 1 84 19 9 TCY H8'A H 1.862 0.000 1 85 19 9 TCY HN6 H 8.489 0.001 1 86 19 9 TCY HN6A H 6.484 0.000 1 87 20 10 F4Q H1' H 6.416 0.001 1 88 20 10 F4Q H2' H 2.917 0.002 1 89 20 10 F4Q H2'' H 2.938 0.001 1 90 20 10 F4Q H4' H 4.820 0.000 1 91 20 10 F4Q H6' H 1.683 0.000 1 92 20 10 F4Q H8 H 7.675 0.001 1 93 20 10 F4Q H8' H 1.071 0.001 1 94 20 10 F4Q H8'' H 1.743 0.000 1 stop_ save_