data_27452 ####################### # Entry information # ####################### save_entry_information _Saveframe_category entry_information _Entry_title ; NMR resonance assignment for the SAM/SAH binding riboswitch RNA bound to S-Adenosylhomocysteine ; _BMRB_accession_number 27452 _BMRB_flat_file_name bmr27452.str _Entry_type original _Submission_date 2018-04-16 _Accession_date 2018-04-16 _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 Weickhmann 'Anna Katharina' . . 2 Keller Heiko . . 3 Duchardt-Ferner Elke . . 4 Wunderlich Christoph H. . 5 Juen Michael . . 6 Kremser Johannes . . 7 Kreutz Christoph . . 8 Woehnert Jens . . stop_ loop_ _Saveframe_category_type _Saveframe_category_type_count assigned_chemical_shifts 2 stop_ loop_ _Data_type _Data_type_count "1H chemical shifts" 318 "13C chemical shifts" 313 "15N chemical shifts" 126 stop_ loop_ _Revision_date _Revision_keyword _Revision_author _Revision_detail 2018-11-07 update BMRB 'update assignments' 2018-10-12 update author 'update assignments' 2018-08-09 original author 'original release' stop_ _Original_release_date 2018-04-16 save_ ############################# # Citation for this entry # ############################# save_entry_citation _Saveframe_category entry_citation _Citation_full . _Citation_title ; NMR resonance assignments for the SAM/SAH-binding riboswitch RNA bound to S-adenosylhomocysteine ; _Citation_status published _Citation_type journal _CAS_abstract_code . _MEDLINE_UI_code . _PubMed_ID 30051308 loop_ _Author_ordinal _Author_family_name _Author_given_name _Author_middle_initials _Author_family_title 1 Weickhmann 'A Katharina' K. . 2 Keller Heiko . . 3 Duchardt-Ferner Elke . . 4 Strebitzer Elisabeth . . 5 Juen Michael A. . 6 Kremser Johannes . . 7 Wurm 'Jan Philip' P. . 8 Kreutz Christoph . . 9 Wohnert Jens . . stop_ _Journal_abbreviation 'Biomol. NMR Assign.' _Journal_name_full 'Biomolecular NMR assignments' _Journal_volume 12 _Journal_issue 2 _Journal_ISSN 1874-270X _Journal_CSD . _Book_chapter_title . _Book_volume . _Book_series . _Book_ISBN . _Conference_state_province . _Conference_abstract_number . _Page_first 329 _Page_last 334 _Year 2018 _Details . loop_ _Keyword NMR-assignment RNA Riboswitch S-Adenosylhomocysteine S-Adenosylmethionine 'Site-specific isotope labeling' 'Triple resonance experiments' stop_ save_ ################################## # Molecular system description # ################################## save_assembly _Saveframe_category molecular_system _Mol_system_name env9b_SAH _Enzyme_commission_number . loop_ _Mol_system_component_name _Mol_label env9b $env9b SAH $entity_SAH 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_env9b _Saveframe_category monomeric_polymer _Mol_type polymer _Mol_polymer_class RNA _Name_common env9b _Molecular_mass . _Mol_thiol_state 'not present' loop_ _Biological_function 'SAM/SAH binding riboswitch' stop_ _Details . ############################## # Polymer residue sequence # ############################## _Residue_count 43 _Mol_residue_sequence ; GUCACAACGGCUUCCUGACG UGGCAGAUUGAAUUAUUGGA GCA ; loop_ _Residue_seq_code _Residue_author_seq_code _Residue_label 1 1 G 2 2 U 3 3 C 4 4 A 5 5 C 6 6 A 7 7 A 8 8 C 9 9 G 10 10 G 11 11 C 12 12 U 13 13 U 14 14 C 15 15 C 16 16 U 17 17 G 18 18 A 19 19 C 20 20 G 21 21 U 22 22 G 23 23 G 24 24 C 25 25 A 26 26 G 27 27 A 28 28 U 29 29 U 30 30 G 31 31 A 32 32 A 33 33 U 34 34 U 35 35 A 36 36 U 37 37 U 38 38 G 39 39 G 40 40 A 41 41 G 42 42 C 43 43 A stop_ _Sequence_homology_query_date . _Sequence_homology_query_revised_last_date . loop_ _Database_name _Database_accession_code _Database_entry_mol_name _Sequence_query_to_submitted_percentage _Sequence_subject_length _Sequence_identity _Sequence_positive _Sequence_homology_expectation_value EMBL RF01727 SAM-SAH . . . . . stop_ save_ ############# # Ligands # ############# save_SAH _Saveframe_category ligand _Mol_type "non-polymer (L-PEPTIDE LINKING)" _Name_common S-ADENOSYL-L-HOMOCYSTEINE _BMRB_code SAH _PDB_code SAH _Molecular_mass 384.411 _Mol_charge 0 _Mol_paramagnetic . _Mol_aromatic yes _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 . ? SD SD S . 0 . ? C C C . 0 . ? O O O . 0 . ? OXT OXT O . 0 . ? C5' C5' C . 0 . ? C4' C4' C . 0 . ? O4' O4' O . 0 . ? C3' C3' C . 0 . ? O3' O3' O . 0 . ? C2' C2' C . 0 . ? O2' O2' O . 0 . ? C1' C1' C . 0 . ? N9 N9 N . 0 . ? C8 C8 C . 0 . ? N7 N7 N . 0 . ? C5 C5 C . 0 . ? C6 C6 C . 0 . ? N6 N6 N . 0 . ? N1 N1 N . 0 . ? C2 C2 C . 0 . ? N3 N3 N . 0 . ? C4 C4 C . 0 . ? HN1 HN1 H . 0 . ? HN2 HN2 H . 0 . ? HA HA H . 0 . ? HB1 HB1 H . 0 . ? HB2 HB2 H . 0 . ? HG1 HG1 H . 0 . ? HG2 HG2 H . 0 . ? HXT HXT H . 0 . ? H5'1 H5'1 H . 0 . ? H5'2 H5'2 H . 0 . ? H4' H4' H . 0 . ? H3' H3' H . 0 . ? HO3' HO3' H . 0 . ? H2' H2' H . 0 . ? HO2' HO2' H . 0 . ? H1' H1' H . 0 . ? H8 H8 H . 0 . ? HN61 HN61 H . 0 . ? HN62 HN62 H . 0 . ? H2 H2 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 HN1 ? ? SING N HN2 ? ? SING CA CB ? ? SING CA C ? ? SING CA HA ? ? SING CB CG ? ? SING CB HB1 ? ? SING CB HB2 ? ? SING CG SD ? ? SING CG HG1 ? ? SING CG HG2 ? ? SING SD C5' ? ? DOUB C O ? ? SING C OXT ? ? SING OXT HXT ? ? SING C5' C4' ? ? SING C5' H5'1 ? ? SING C5' H5'2 ? ? SING C4' O4' ? ? SING C4' C3' ? ? SING C4' H4' ? ? SING O4' C1' ? ? SING C3' O3' ? ? SING C3' C2' ? ? SING C3' H3' ? ? SING O3' HO3' ? ? SING C2' O2' ? ? SING C2' C1' ? ? SING C2' H2' ? ? SING O2' HO2' ? ? SING C1' N9 ? ? SING C1' H1' ? ? SING N9 C8 ? ? SING N9 C4 ? ? DOUB C8 N7 ? ? SING C8 H8 ? ? SING N7 C5 ? ? SING C5 C6 ? ? DOUB C5 C4 ? ? SING C6 N6 ? ? DOUB C6 N1 ? ? SING N6 HN61 ? ? SING N6 HN62 ? ? SING N1 C2 ? ? DOUB C2 N3 ? ? SING C2 H2 ? ? SING N3 C4 ? ? stop_ _Mol_thiol_state . _Sequence_homology_query_date . save_ #################### # Natural source # #################### save_natural_source _Saveframe_category natural_source loop_ _Mol_label _Organism_name_common _NCBI_taxonomy_ID _Superkingdom _Kingdom _Genus _Species _Details $env9b . . . . . . 'marine environmental sample' 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 $env9b 'recombinant technology' . Escherichia coli . pSP64 stop_ save_ ##################################### # Sample contents and methodology # ##################################### ######################## # Sample description # ######################## save_13C15N _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 710 uM '[U-13C; U-15N]' S-Adenosylhomocysteine 2 mM 'natural abundance' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ save_15N _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 910 uM [U-15N] S-Adenosylhomocysteine 2.5 mM 'natural abundance' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ save_13C15N-U _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 800 uM '[U-13C; U-15N]-Ura' S-Adenosylhomocysteine 1.6 mM 'natural abundance' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ save_seldeut _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 750 uM '[U-5-D1/ribose-3 ,4 ,5 ,5 -D4]' S-Adenosylhomocysteine 3 mM 'natural abundance' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ save_13C15N-SAH _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 700 uM 'natural abundance' S-Adenosylhomocysteine 0.5 mM '[U-13C; U-15N]' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ save_13C15N-AC _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 800 uM '[U-13C; U-15N]-Ade, [U-13C; U-15N]-Ade' S-Adenosylhomocysteine 2 mM 'natural abundance' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ save_13C15N-G _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 850 uM '[U-13C; U-15N]-Gua' S-Adenosylhomocysteine 2 mM 'natural abundance' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ save_unlab _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 1.2 uM 'natural abundance' S-Adenosylhomocysteine 4 mM 'natural abundance' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ save_13C15N-AC_D2O _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 800 uM '[U-13C; U-15N]-Ade, [U-13C; U-15N]-Ade' S-Adenosylhomocysteine 2 mM 'natural abundance' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ save_13C15N-U_D2O _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 800 uM '[U-13C; U-15N]-Ura' S-Adenosylhomocysteine 1.6 mM 'natural abundance' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ save_13C15N-G_D2O _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 850 uM '[U-13C; U-15N]-Gua' S-Adenosylhomocysteine 2 mM 'natural abundance' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ save_13C15N-U_13C15N-SAH _Saveframe_category sample _Sample_type solution _Details . loop_ _Mol_label _Concentration_value _Concentration_value_units _Isotopic_labeling $env9b 480 uM '[U-13C; U-15N]-Ura' S-Adenosylhomocysteine 750 mM '[U-13C; U-15N]' 'potassium phosphate' 25 mM 'natural abundance' 'potassium chloride' 50 mM 'natural abundance' 'magnesium acetate' 2 mM 'natural abundance' stop_ save_ ############################ # Computer software used # ############################ save_TOPSPIN _Saveframe_category software _Name TOPSPIN _Version '3.2 or 3.5' loop_ _Vendor _Address _Electronic_address Bruker . . stop_ loop_ _Task processing stop_ _Details . save_ save_CARA _Saveframe_category software _Name CARA _Version 1.9.1b9 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 950 _Details . save_ save_spectrometer_2 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 900 _Details . save_ save_spectrometer_3 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 800 _Details . save_ save_spectrometer_4 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 700 _Details . save_ save_spectrometer_5 _Saveframe_category NMR_spectrometer _Manufacturer Bruker _Model Avance _Field_strength 600 _Details . save_ ############################# # NMR applied experiments # ############################# save_2D_1H-15N_HSQC_1 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $13C15N save_ save_2D_1H-15N_HSQC_2 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $13C15N-U save_ save_2D_1H-15N_HSQC_3 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $13C15N-AC save_ save_2D_1H-15N_HSQC_4 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $13C15N-G save_ save_2D_1H-15N_HSQC_NH2_only_5 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC NH2 only' _Sample_label $15N save_ save_2D_1H-13C_HSQC_aliphatic_6 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $13C15N save_ save_2D_1H-13C_HSQC_aliphatic_7 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $13C15N-AC save_ save_2D_1H-13C_HSQC_aliphatic_8 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $13C15N-U save_ save_2D_1H-13C_HSQC_aliphatic_9 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $13C15N-G save_ save_2D_1H-13C_HSQC_aromatic_10 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aromatic' _Sample_label $13C15N save_ save_2D_1H-13C_HSQC_aromatic_11 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aromatic' _Sample_label $13C15N-AC save_ save_2D_1H-13C_HSQC_aromatic_12 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aromatic' _Sample_label $13C15N-U save_ save_2D_1H-13C_HSQC_aromatic_13 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aromatic' _Sample_label $13C15N-G save_ save_2D_1H-1H_NOESY_14 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $unlab save_ save_3D_1H-13C_NOESY_aromatic_15 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-13C NOESY aromatic' _Sample_label $13C15N-AC save_ save_3D_1H-13C_NOESY_aromatic_16 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-13C NOESY aromatic' _Sample_label $13C15N-U save_ save_3D_1H-13C_NOESY_aromatic_17 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-13C NOESY aromatic' _Sample_label $13C15N-G save_ save_3D_1H-13C_NOESY_aliphatic_18 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-13C NOESY aliphatic' _Sample_label $13C15N-AC_D2O save_ save_3D_1H-13C_NOESY_aliphatic_19 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-13C NOESY aliphatic' _Sample_label $13C15N-U_D2O save_ save_3D_1H-13C_NOESY_aliphatic_20 _Saveframe_category NMR_applied_experiment _Experiment_name '3D 1H-13C NOESY aliphatic' _Sample_label $13C15N-G_D2O save_ save_2D_1H-1H_NOESY_21 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-1H NOESY' _Sample_label $unlab save_ save_3D_HCCH-TOCSY_22 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-TOCSY' _Sample_label $13C15N-AC_D2O save_ save_3D_HCCH-COSY_23 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-COSY' _Sample_label $13C15N-AC_D2O save_ save_3D_HCCH-TOCSY_24 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-TOCSY' _Sample_label $13C15N-U_D2O save_ save_3D_HCCH-COSY_25 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-COSY' _Sample_label $13C15N-U_D2O save_ save_3D_HCCH-TOCSY_26 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-TOCSY' _Sample_label $13C15N-G_D2O save_ save_3D_HCCH-COSY_27 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-COSY' _Sample_label $13C15N-G_D2O save_ save_1D_1H-HS11ECHO_28 _Saveframe_category NMR_applied_experiment _Experiment_name '1D 1H-HS11ECHO' _Sample_label $unlab save_ save_2D_1H-15N_HNN-COSY_29 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HNN-COSY' _Sample_label $13C15N save_ save_2D_1H-13C_HNCO_30 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HNCO' _Sample_label $13C15N-G save_ save_2D_1H-13C_HNCO_31 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HNCO' _Sample_label $13C15N-U save_ save_2D_1H-13C_H5C5(C4N)H_32 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C H5C5(C4N)H' _Sample_label $13C15N-AC save_ save_2D_1H-15N_HCN_aromatic_33 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HCN aromatic' _Sample_label $13C15N-U save_ save_2D_1H-15N_HCN_aliphatic_34 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HCN aliphatic' _Sample_label $13C15N-U_D2O save_ save_2D_1H-15N_2bond-HSQC_35 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N 2bond-HSQC' _Sample_label $15N save_ save_TROSY_relayed_HCCH-COSY_36 _Saveframe_category NMR_applied_experiment _Experiment_name 'TROSY relayed HCCH-COSY' _Sample_label $13C15N-AC_D2O save_ save_2D_1H-13C_long-rangeH8(C8)C5(N1)H1_37 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C long-rangeH8(C8)C5(N1)H1' _Sample_label $13C15N-G save_ save_2D_1H-13C_H5C5(C4N)H_38 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C H5C5(C4N)H' _Sample_label $13C15N-U save_ save_2D_1H-15N_HCN_aromatic_39 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HCN aromatic' _Sample_label $13C15N-AC save_ save_2D_1H-15N_HCN_aliphatic_40 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HCN aliphatic' _Sample_label $13C15N-AC_D2O save_ save_2D_1H-15N_HCN_aromatic_41 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HCN aromatic' _Sample_label $13C15N-G save_ save_2D_1H-15N_HCN_aliphatic_42 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HCN aliphatic' _Sample_label $13C15N-G_D2O save_ save_2D_1H-15N_HNN-COSY_43 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HNN-COSY' _Sample_label $13C15N-U_13C15N-SAH save_ save_2D_1H-15N_HSQC_44 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-15N HSQC' _Sample_label $15N save_ save_2D_lr-1H,15N-HSQC_45 _Saveframe_category NMR_applied_experiment _Experiment_name '2D lr-1H,15N-HSQC' _Sample_label $15N save_ save_2D_1H-13C_HSQC_aliphatic_46 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aliphatic' _Sample_label $13C15N-SAH save_ save_2D_1H-13C_HSQC_aromatic_47 _Saveframe_category NMR_applied_experiment _Experiment_name '2D 1H-13C HSQC aromatic' _Sample_label $13C15N-SAH save_ save_3D_HCCH-COSY_48 _Saveframe_category NMR_applied_experiment _Experiment_name '3D HCCH-COSY' _Sample_label $13C15N-SAH save_ ####################### # Sample conditions # ####################### save_298K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 75 . mM pH 6.2 . pH pressure 1 . atm temperature 298 . K stop_ save_ save_283K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 75 . mM pH 6.2 . pH pressure 1 . atm temperature 283 . K stop_ save_ save_271K _Saveframe_category sample_conditions _Details . loop_ _Variable_type _Variable_value _Variable_value_error _Variable_value_units 'ionic strength' 75 . mM pH 6.2 . pH pressure 1 . atm temperature 271 . 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 external indirect . . . 0.251449530 DSS H 1 'methyl protons' ppm 0.00 external direct . . . 1.000000000 DSS N 15 'methyl protons' ppm 0.00 external indirect . . . 0.101329118 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_1 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-15N HSQC NH2 only' '2D 1H-13C HSQC aliphatic' '2D 1H-13C HSQC aromatic' '2D 1H-1H NOESY' '3D 1H-13C NOESY aromatic' '3D 1H-13C NOESY aliphatic' '3D HCCH-TOCSY' '3D HCCH-COSY' '1D 1H-HS11ECHO' '2D 1H-15N HNN-COSY' '2D 1H-13C HNCO' '2D 1H-13C H5C5(C4N)H' '2D 1H-15N HCN aromatic' '2D 1H-15N HCN aliphatic' '2D 1H-15N 2bond-HSQC' 'TROSY relayed HCCH-COSY' '2D 1H-13C long-rangeH8(C8)C5(N1)H1' '2D lr-1H,15N-HSQC' stop_ loop_ _Sample_label $13C15N $13C15N-U $13C15N-AC $13C15N-G $15N $unlab $13C15N-AC_D2O $13C15N-U_D2O $13C15N-G_D2O $13C15N-U_13C15N-SAH $13C15N-SAH stop_ _Sample_conditions_label $298K _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name env9b _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 G H1 H 12.616 0.02 1 2 1 1 G H1' H 5.515 0.02 1 3 1 1 G H2' H 4.666 0.02 1 4 1 1 G H3' H 4.121 0.02 1 5 1 1 G H4' H 4.319 0.02 1 6 1 1 G H8 H 7.995 0.02 1 7 1 1 G C1' C 85.710 0.3 1 8 1 1 G C2 C 150.886 0.3 1 9 1 1 G C2' C 70.629 0.3 1 10 1 1 G C3' C 67.58 0.3 1 11 1 1 G C4' C 78.786 0.3 1 12 1 1 G C5 C 78.786 0.3 1 13 1 1 G C6 C 156.067 0.3 1 14 1 1 G C8 C 134.235 0.3 1 15 1 1 G N1 N 146.361 0.3 1 16 1 1 G N7 N 230.411 0.3 1 17 1 1 G N9 N 167.552 0.3 1 18 2 2 U H1' H 5.368 0.02 1 19 2 2 U H2' H 3.927 0.02 1 20 2 2 U H3 H 12.149 0.02 1 21 2 2 U H3' H 4.396 0.02 1 22 2 2 U H4' H 4.39 0.02 1 23 2 2 U H5 H 5.302 0.02 1 24 2 2 U H6 H 7.766 0.3 1 25 2 2 U C1' C 87.95 0.3 1 26 2 2 U C2 C 149.012 0.3 1 27 2 2 U C2' C 70.116 0.3 1 28 2 2 U C3' C 71.927 0.3 1 29 2 2 U C4 C 161.371 0.3 1 30 2 2 U C5 C 99.544 0.3 1 31 2 2 U C6 C 135.939 0.3 1 32 2 2 U N3 N 157.766 0.3 1 33 3 3 C H1' H 5.362 0.02 1 34 3 3 C H2' H 4.161 0.02 1 35 3 3 C H3' H 4.406 0.02 1 36 3 3 C H5 H 5.45 0.02 1 37 3 3 C H6 H 7.742 0.02 1 38 3 3 C H41 H 8.246 0.02 2 39 3 3 C H42 H 6.817 0.02 2 40 3 3 C C1' C 87.854 0.3 1 41 3 3 C C2' C 69.939 0.3 1 42 3 3 C C3' C 66.76 0.3 1 43 3 3 C C5 C 92.004 0.3 1 44 3 3 C C6 C 136.75 0.3 1 45 3 3 C N1 N 150.874 0.3 1 46 3 3 C N3 N 195.158 0.3 1 47 3 3 C N4 N 97.947 0.3 1 48 4 4 A H1' H 5.618 0.02 1 49 4 4 A H2 H 7.138 0.02 1 50 4 4 A H2' H 4.282 0.02 1 51 4 4 A H3' H 3.903 0.02 1 52 4 4 A H4' H 4.191 0.02 2 53 4 4 A H8 H 7.73 0.02 1 54 4 4 A H61 H 7.918 0.02 2 55 4 4 A H62 H 6.058 0.02 1 56 4 4 A C1' C 87.184 0.3 1 57 4 4 A C2 C 147.681 0.3 1 58 4 4 A C2' C 70.137 0.3 1 59 4 4 A C3' C 67.293 0.3 1 60 4 4 A C4 C 143.046 0.3 1 61 4 4 A C4' C 76.542 0.3 1 62 4 4 A C6 C 153.716 0.3 1 63 4 4 A C8 C 133.746 0.3 1 64 4 4 A N1 N 220.725 0.3 1 65 4 4 A N3 N 211.993 0.3 1 66 4 4 A N6 N 84.334 0.3 1 67 4 4 A N7 N 229.598 0.3 1 68 4 4 A N9 N 169.827 0.3 1 69 5 5 C H1' H 4.86 0.02 1 70 5 5 C H2' H 4.259 0.02 1 71 5 5 C H3' H 4.188 0.02 1 72 5 5 C H5 H 4.665 0.02 1 73 5 5 C H6 H 6.815 0.02 1 74 5 5 C H41 H 6.836 0.02 2 75 5 5 C H42 H 6.095 0.02 2 76 5 5 C C1' C 88.529 0.3 1 77 5 5 C C2' C 69.971 0.3 1 78 5 5 C C3' C 66.505 0.3 1 79 5 5 C C5 C 91.026 0.3 1 80 5 5 C C6 C 134.182 0.3 1 81 5 5 C N1 N 148.916 0.3 1 82 5 5 C N3 N 194.553 0.3 1 83 5 5 C N4 N 95.957 0.3 1 84 6 6 A H1' H 5.487 0.02 1 85 6 6 A H2 H 7.033 0.02 1 86 6 6 A H2' H 3.994 0.02 1 87 6 6 A H3' H 4.876 0.02 1 88 6 6 A H4' H 4.349 0.02 1 89 6 6 A H8 H 8.132 0.02 1 90 6 6 A C1' C 87.694 0.3 1 91 6 6 A C2 C 149.491 0.3 1 92 6 6 A C2' C 72.077 0.3 1 93 6 6 A C3' C 68.809 0.3 1 94 6 6 A C4 C 143.478 0.3 1 95 6 6 A C4' C 77.161 0.3 1 96 6 6 A C6 C 153.014 0.3 1 97 6 6 A C8 C 134.77 0.3 1 98 6 6 A N1 N 223.619 0.3 1 99 6 6 A N3 N 213.802 0.3 1 100 6 6 A N7 N 229.215 0.3 1 101 6 6 A N9 N 170.426 0.3 1 102 7 7 A H1' H 5.863 0.02 1 103 7 7 A H2 H 7.999 0.02 1 104 7 7 A H2' H 4.779 0.02 1 105 7 7 A H3' H 4.485 0.02 1 106 7 7 A H4' H 4.385 0.02 1 107 7 7 A H8 H 7.964 0.02 1 108 7 7 A C1' C 88.193 0.3 1 109 7 7 A C2 C 148.472 0.3 1 110 7 7 A C2' C 70.262 0.3 1 111 7 7 A C3' C 67.075 0.3 1 112 7 7 A C4 C 142.912 0.3 1 113 7 7 A C4' C 77.955 0.3 1 114 7 7 A C6 C 154.691 0.3 1 115 7 7 A C8 C 135.849 0.3 1 116 7 7 A N1 N 221.403 0.3 1 117 7 7 A N3 N 216.215 0.3 1 118 7 7 A N7 N 236.629 0.3 1 119 7 7 A N9 N 168.245 0.3 1 120 8 8 C H1' H 4.913 0.02 1 121 8 8 C H2' H 3.895 0.02 1 122 8 8 C H3' H 4.492 0.02 1 123 8 8 C H4' H 4.099 0.02 1 124 8 8 C H5 H 5.56 0.02 1 125 8 8 C H6 H 7.545 0.02 1 126 8 8 C H41 H 7.429 0.02 2 127 8 8 C H42 H 6.372 0.02 2 128 8 8 C C1' C 88.7 0.3 1 129 8 8 C C2' C 71.716 0.3 1 130 8 8 C C3' C 67.163 0.3 1 131 8 8 C C4' C 77.527 0.3 1 132 8 8 C C5 C 93.488 0.3 1 133 8 8 C C6 C 135.18 0.3 1 134 8 8 C N1 N 151.067 0.3 1 135 8 8 C N3 N 200.119 0.3 1 136 8 8 C N4 N 94.612 0.3 1 137 9 9 G H1 H 10.845 0.02 1 138 9 9 G H1' H 5.594 0.02 1 139 9 9 G H2' H 4.503 0.02 1 140 9 9 G H3' H 4.608 0.02 1 141 9 9 G H4' H 4.329 0.02 1 142 9 9 G H5' H 4.117 0.02 2 143 9 9 G H5'' H 3.918 0.02 2 144 9 9 G H8 H 7.958 0.02 1 145 9 9 G C1' C 80.124 0.3 1 146 9 9 G C2 C 151.583 0.3 1 147 9 9 G C2' C 67.715 0.3 1 148 9 9 G C3' C 71.176 0.3 1 149 9 9 G C4' C 81.415 0.3 1 150 9 9 G C5 C 115.007 0.3 1 151 9 9 G C5' C 61.94 0.3 1 152 9 9 G C6 C 155.376 0.3 1 153 9 9 G C8 C 131.747 0.3 1 154 9 9 G N1 N 148.069 0.3 1 155 9 9 G N7 N 236.52 0.3 1 156 9 9 G N9 N 162.81 0.3 1 157 10 10 G H1 H 12.61 0.02 1 158 10 10 G H1' H 5.672 0.02 1 159 10 10 G H2' H 4.646 0.02 1 160 10 10 G H3' H 4.716 0.02 1 161 10 10 G H4' H 4.361 0.02 1 162 10 10 G H5' H 4.384 0.02 2 163 10 10 G H5'' H 4.056 0.02 2 164 10 10 G H8 H 8.148 0.02 1 165 10 10 G C1' C 89.256 0.3 1 166 10 10 G C2 C 151.177 0.3 1 167 10 10 G C2' C 69.455 0.3 1 168 10 10 G C3' C 67.073 0.3 1 169 10 10 G C4' C 78.474 0.3 1 170 10 10 G C5 C 115.686 0.3 1 171 10 10 G C5' C 59.064 0.3 1 172 10 10 G C6 C 156.754 0.3 1 173 10 10 G C8 C 134.571 0.3 1 174 10 10 G N1 N 147.146 0.3 1 175 10 10 G N7 N 229.664 0.3 1 176 10 10 G N9 N 167.344 0.3 1 177 11 11 C H1' H 5.378 0.02 1 178 11 11 C H2' H 3.866 0.02 1 179 11 11 C H3' H 4.338 0.02 1 180 11 11 C H4' H 4.185 0.02 1 181 11 11 C H5 H 5.196 0.02 1 182 11 11 C H5' H 3.922 0.02 2 183 11 11 C H5'' H 3.922 0.02 2 184 11 11 C H6 H 7.391 0.02 1 185 11 11 C H41 H 7.995 0.02 2 186 11 11 C H42 H 6.52 0.02 2 187 11 11 C C1' C 88.695 0.3 1 188 11 11 C C2' C 70.029 0.3 1 189 11 11 C C3' C 66.398 0.3 1 190 11 11 C C4' C 76.325 0.3 1 191 11 11 C C5 C 93.426 0.3 1 192 11 11 C C5' C 58.917 0.3 1 193 11 11 C C6 C 134.89 0.3 1 194 11 11 C N1 N 149.51 0.3 1 195 11 11 C N3 N 196.184 0.3 1 196 11 11 C N4 N 99.878 0.3 1 197 12 12 U H1' H 5.879 0.02 1 198 12 12 U H2' H 4.275 0.02 1 199 12 12 U H3 H 12.907 0.02 1 200 12 12 U H3' H 4.634 0.02 1 201 12 12 U H4' H 4.306 0.02 1 202 12 12 U H5 H 4.025 0.02 1 203 12 12 U H6 H 7.356 0.02 1 204 12 12 U C1' C 83.654 0.3 1 205 12 12 U C2 C 148.598 0.3 1 206 12 12 U C2' C 69.86 0.3 1 207 12 12 U C3' C 73.904 0.3 1 208 12 12 U C4 C 161.289 0.3 1 209 12 12 U C4' C 80.759 0.3 1 210 12 12 U C5 C 99.864 0.3 1 211 12 12 U C6 C 135.88 0.3 1 212 12 12 U N1 N 138.691 0.3 1 213 12 12 U N3 N 158.421 0.3 1 214 13 13 U H1' H 6.025 0.02 1 215 13 13 U H2' H 4.416 0.02 1 216 13 13 U H3' H 4.625 0.02 1 217 13 13 U H4' H 4.424 0.02 1 218 13 13 U H5 H 5.869 0.02 1 219 13 13 U H6 H 7.847 0.02 1 220 13 13 U C1' C 84.326 0.3 1 221 13 13 U C2' C 70.185 0.3 1 222 13 13 U C3' C 72.306 0.3 1 223 13 13 U C4' C 80.567 0.3 1 224 13 13 U C5 C 100.232 0.3 1 225 13 13 U C6 C 138.33 0.3 1 226 13 13 U N1 N 142.496 0.3 1 227 14 14 C H1' H 5.498 0.02 1 228 14 14 C H2' H 4.349 0.02 1 229 14 14 C H3' H 4.348 0.02 1 230 14 14 C H5 H 5.825 0.02 1 231 14 14 C H6 H 7.824 0.02 1 232 14 14 C H41 H 8.6 0.02 2 233 14 14 C H42 H 6.126 0.02 2 234 14 14 C C1' C 89.113 0.3 1 235 14 14 C C2' C 70.074 0.3 1 236 14 14 C C3' C 66.945 0.3 1 237 14 14 C C5 C 93.598 0.3 1 238 14 14 C C6 C 136.55 0.3 1 239 14 14 C N1 N 149.941 0.3 1 240 14 14 C N3 N 196.222 0.3 1 241 14 14 C N4 N 100.196 0.3 1 242 15 15 C H1' H 5.239 0.02 1 243 15 15 C H2' H 4.19 0.02 1 244 15 15 C H3' H 4.347 0.02 1 245 15 15 C H5 H 5.384 0.02 1 246 15 15 C H6 H 7.543 0.02 1 247 15 15 C H41 H 8.411 0.02 2 248 15 15 C H42 H 6.792 0.02 2 249 15 15 C C1' C 89.37 0.3 1 250 15 15 C C2' C 69.518 0.3 1 251 15 15 C C3' C 66.591 0.3 1 252 15 15 C C5 C 92.343 0.3 1 253 15 15 C C6 C 135.372 0.3 1 254 15 15 C N1 N 148.789 0.3 1 255 15 15 C N3 N 196.069 0.3 1 256 15 15 C N4 N 99.774 0.3 1 257 16 16 U H1' H 5.301 0.02 1 258 16 16 U H2' H 4.42 0.02 1 259 16 16 U H3 H 13.52 0.02 1 260 16 16 U H3' H 4.388 0.02 1 261 16 16 U H4' H 4.282 0.02 1 262 16 16 U H5 H 5.219 0.02 1 263 16 16 U H6 H 7.763 0.02 1 264 16 16 U C1' C 87.355 0.3 1 265 16 16 U C2 C 147.996 0.3 1 266 16 16 U C2' C 69.67 0.3 1 267 16 16 U C3' C 66.373 0.3 1 268 16 16 U C4 C 162.167 0.3 1 269 16 16 U C4' C 76.36 0.3 1 270 16 16 U C5 C 97.888 0.3 1 271 16 16 U C6 C 135.24 0.3 1 272 16 16 U N3 N 160.201 0.3 1 273 17 17 G H1 H 12.021 0.02 1 274 17 17 G H1' H 5.642 0.02 1 275 17 17 G H2' H 3.993 0.02 1 276 17 17 G H3' H 4.352 0.02 1 277 17 17 G H4' H 4.259 0.02 1 278 17 17 G H8 H 7.164 0.02 1 279 17 17 G H21 H 7.973 0.02 2 280 17 17 G C1' C 88.414 0.3 1 281 17 17 G C2 C 150.249 0.3 1 282 17 17 G C2' C 70.622 0.3 1 283 17 17 G C3' C 66.583 0.3 1 284 17 17 G C4' C 76.576 0.3 1 285 17 17 G C5 C 112.818 0.3 1 286 17 17 G C6 C 154.496 0.3 1 287 17 17 G C8 C 128.331 0.3 1 288 17 17 G N1 N 144.192 0.3 1 289 17 17 G N2 N 75.603 0.3 1 290 17 17 G N7 N 235.847 0.3 1 291 17 17 G N9 N 168.145 0.3 1 292 18 18 A H1' H 5.072 0.02 1 293 18 18 A H2 H 8.449 0.02 1 294 18 18 A H2' H 3.962 0.02 1 295 18 18 A H3' H 4.203 0.02 1 296 18 35 A H5' H 3.736 0.02 2 297 18 35 A H5'' H 3.621 0.02 2 298 18 18 A H8 H 7.667 0.02 1 299 18 18 A C1' C 83.815 0.3 1 300 18 18 A C2 C 150.926 0.3 1 301 18 18 A C2' C 73.928 0.3 1 302 18 18 A C3' C 72.299 0.3 1 303 35 35 A C5' C 61.485 0.3 1 304 18 18 A C4 C 144.88 0.3 1 305 18 18 A C8 C 134.88 0.3 1 306 18 18 A N3 N 216.495 0.3 1 307 18 18 A N7 N 234.515 0.3 1 308 18 18 A N9 N 166.757 0.3 1 309 19 19 C H1' H 4.696 0.02 1 310 19 19 C H2' H 4.402 0.02 1 311 19 19 C H3' H 4.12 0.02 1 312 19 19 C H4' H 4.346 0.02 1 313 19 19 C H5 H 4.821 0.02 1 314 19 19 C H6 H 7.199 0.02 1 315 19 19 C H41 H 7.347 0.02 2 316 19 19 C H42 H 6.244 0.02 2 317 19 19 C C1' C 88.123 0.3 1 318 19 19 C C2' C 70.189 0.3 1 319 19 19 C C3' C 66.353 0.3 1 320 19 19 C C4' C 77.202 0.3 1 321 19 19 C C5 C 91.131 0.3 1 322 19 19 C C6 C 136.042 0.3 1 323 19 19 C N1 N 150.95 0.3 1 324 19 19 C N3 N 198.498 0.3 1 325 19 19 C N4 N 94.607 0.3 1 326 20 20 G H1 H 12.793 0.02 1 327 20 20 G H1' H 5.164 0.02 1 328 20 20 G H2' H 4.124 0.02 1 329 20 20 G H3' H 4.454 0.02 1 330 20 20 G H4' H 4.268 0.02 1 331 20 20 G H8 H 7.491 0.02 1 332 20 20 G H21 H 8.671 0.02 2 333 20 20 G H22 H 6.509 0.02 2 334 20 20 G C1' C 87.84 0.3 1 335 20 20 G C2 C 151.07 0.3 1 336 20 20 G C2' C 69.481 0.3 1 337 20 20 G C3' C 68.133 0.3 1 338 20 20 G C4' C 76.307 0.3 1 339 20 20 G C5 C 113.962 0.3 1 340 20 20 G C6 C 156.42 0.3 1 341 20 20 G C8 C 132.644 0.3 1 342 20 20 G N1 N 147.198 0.3 1 343 20 20 G N2 N 75.546 0.3 1 344 20 20 G N7 N 222.345 0.3 1 345 20 20 G N9 N 168.67 0.3 1 346 21 21 U H1' H 5.399 0.02 1 347 21 21 U H2' H 4.448 0.02 1 348 21 21 U H3 H 13.466 0.02 1 349 21 21 U H3' H 4.434 0.02 1 350 21 21 U H4' H 4.282 0.02 1 351 21 21 U H5 H 4.84 0.02 1 352 21 21 U H6 H 7.746 0.02 1 353 21 21 U C1' C 88.205 0.3 1 354 21 21 U C2 C 146.992 0.3 1 355 21 21 U C2' C 69.778 0.3 1 356 21 21 U C3' C 66.508 0.3 1 357 21 21 U C4 C 164.291 0.3 1 358 21 21 U C4' C 76.518 0.3 1 359 21 21 U C5 C 98.175 0.3 1 360 21 21 U C6 C 136.573 0.3 1 361 21 21 U N1 N 142.474 0.3 1 362 21 21 U N3 N 160.73 0.3 1 363 22 22 G H1 H 11.957 0.02 1 364 22 22 G H1' H 5.673 0.02 1 365 22 22 G H2' H 4.275 0.02 1 366 22 22 G H3' H 4.453 0.02 1 367 22 22 G H4' H 4.343 0.02 1 368 22 22 G H5' H 4.33 0.02 2 369 22 22 G H5'' H 3.991 0.02 2 370 22 22 G H8 H 7.582 0.02 1 371 22 22 G H21 H 7.205 0.02 2 372 22 22 G C1' C 86.523 0.3 1 373 22 22 G C2 C 150.174 0.3 1 374 22 22 G C2' C 70.4 0.3 1 375 22 22 G C3' C 67.704 0.3 1 376 22 22 G C4' C 76.566 0.3 1 377 22 22 G C5 C 115.366 0.3 1 378 22 22 G C5' C 60.269 0.3 1 379 22 22 G C6 C 156.304 0.3 1 380 22 22 G C8 C 130.95 0.3 1 381 22 22 G N1 N 146.288 0.3 1 382 22 22 G N2 N 72.351 0.3 1 383 22 22 G N7 N 233.759 0.3 1 384 22 22 G N9 N 168.396 0.3 1 385 23 23 G H1 H 11.284 0.02 1 386 23 23 G H1' H 5.52 0.02 1 387 23 23 G H2' H 4.352 0.02 1 388 23 23 G H3' H 4.146 0.02 1 389 23 23 G H4' H 4.288 0.02 1 390 23 23 G H8 H 7.076 0.02 1 391 23 23 G H21 H 6.141 0.02 2 392 23 23 G H22 H 6.141 0.02 2 393 23 23 G C1' C 87.685 0.3 1 394 23 23 G C2 C 150.053 0.3 1 395 23 23 G C2' C 69.859 0.3 1 396 23 23 G C3' C 67.34 0.3 1 397 23 23 G C4' C 76.687 0.3 1 398 23 23 G C5 C 114.709 0.3 1 399 23 23 G C6 C 155.493 0.3 1 400 23 23 G C8 C 131.092 0.3 1 401 23 23 G N1 N 143.897 0.3 1 402 23 23 G N2 N 71.957 0.3 1 403 23 23 G N7 N 231.768 0.3 1 404 23 23 G N9 N 168.675 0.3 1 405 24 24 C H1' H 5.25 0.02 1 406 24 24 C H2' H 4.275 0.02 1 407 24 24 C H3' H 3.915 0.02 1 408 24 24 C H5 H 5.096 0.02 1 409 24 24 C H6 H 7.362 0.02 1 410 24 24 C H41 H 7.898 0.02 2 411 24 24 C H42 H 6.678 0.02 2 412 24 24 C C1' C 88.021 0.3 1 413 24 24 C C2' C 70.058 0.3 1 414 24 24 C C3' C 67.385 0.3 1 415 24 24 C C5 C 91.992 0.3 1 416 24 24 C C6 C 134.292 0.3 1 417 24 24 C N1 N 149.767 0.3 1 418 24 24 C N3 N 194.768 0.3 1 419 24 24 C N4 N 98.313 0.3 1 420 25 25 A H1' H 5.665 0.02 1 421 25 25 A H2 H 6.878 0.02 1 422 25 25 A H2' H 4.339 0.02 1 423 25 25 A H3' H 4.302 0.02 1 424 25 25 A H8 H 7.608 0.02 1 425 25 25 A C1' C 87.838 0.3 1 426 25 25 A C2 C 148.087 0.3 1 427 25 25 A C2' C 70.095 0.3 1 428 25 25 A C3' C 67.754 0.3 1 429 25 25 A C4 C 143.1 0.3 1 430 25 25 A C6 C 152.852 0.3 1 431 25 25 A C8 C 133.893 0.3 1 432 25 25 A N1 N 223.701 0.3 1 433 25 25 A N3 N 214.314 0.3 1 434 25 25 A N7 N 230.259 0.3 1 435 25 25 A N9 N 168.716 0.3 1 436 26 26 G H1' H 5.03 0.02 1 437 26 26 G H2' H 4.172 0.02 1 438 26 26 G H3' H 4.336 0.02 1 439 26 26 G H4' H 4.138 0.02 1 440 26 26 G H5' H 4.158 0.02 2 441 26 26 G H5'' H 3.872 0.02 2 442 26 26 G H8 H 7.22 0.02 1 443 26 26 G C1' C 86.168 0.3 1 444 26 26 G C2' C 69.769 0.3 1 445 26 26 G C3' C 69.11 0.3 1 446 26 26 G C4' C 77.752 0.3 1 447 26 26 G C5' C 60.441 0.3 1 448 26 26 G C8 C 132.149 0.3 1 449 26 26 G N7 N 234.343 0.3 1 450 26 26 G N9 N 167.257 0.3 1 451 27 27 A H1' H 5.756 0.02 1 452 27 27 A H2 H 7.954 0.02 1 453 27 27 A H2' H 4.348 0.02 1 454 27 27 A H3' H 4.479 0.02 1 455 27 27 A H4' H 4.276 0.02 1 456 27 27 A H5' H 4.151 0.02 2 457 27 27 A H5'' H 3.889 0.02 2 458 27 27 A H8 H 7.914 0.02 1 459 27 27 A C1' C 85.619 0.3 1 460 27 27 A C2 C 149.812 0.3 1 461 27 27 A C2' C 70.644 0.3 1 462 27 27 A C3' C 67.144 0.3 1 463 27 27 A C4 C 144.476 0.3 1 464 27 27 A C4' C 78.825 0.3 1 465 27 27 A C5' C 61.071 0.3 1 466 27 27 A C6 C 153.877 0.3 1 467 27 27 A C8 C 135.438 0.3 1 468 27 27 A N1 N 224.934 0.3 1 469 27 27 A N3 N 215.077 0.3 1 470 27 27 A N7 N 230.88 0.3 1 471 27 27 A N9 N 168.4 0.3 1 472 28 28 U H1' H 5.549 0.02 1 473 28 28 U H2' H 4.072 0.02 1 474 28 28 U H3' H 4.394 0.02 1 475 28 28 U H5 H 5.353 0.02 1 476 28 28 U H6 H 7.43 0.02 1 477 28 28 U C1' C 85.19 0.3 1 478 28 28 U C2' C 70.159 0.3 1 479 28 28 U C3' C 71.336 0.3 1 480 28 28 U C5 C 99.003 0.3 1 481 28 28 U C6 C 137.512 0.3 1 482 28 28 U N1 N 142.493 0.3 1 483 29 29 U H1' H 5.652 0.02 1 484 29 29 U H2' H 4.148 0.02 1 485 29 29 U H3' H 4.394 0.02 1 486 29 29 U H4' H 4.183 0.02 1 487 29 29 U H5 H 5.612 0.02 1 488 29 29 U H6 H 7.528 0.02 1 489 29 29 U C1' C 85.336 0.3 1 490 29 29 U C2' C 70.232 0.3 1 491 29 29 U C3' C 71.504 0.3 1 492 29 29 U C4' C 79.286 0.3 1 493 29 29 U C5 C 99.504 0.3 1 494 29 29 U C6 C 138.014 0.3 1 495 29 29 U N1 N 142.828 0.3 1 496 30 30 G H1' H 5.525 0.02 1 497 30 30 G H2' H 4.602 0.02 1 498 30 30 G H3' H 4.497 0.02 1 499 30 30 G H8 H 7.778 0.02 1 500 30 30 G C1' C 85.502 0.3 1 501 30 30 G C2' C 70.19 0.3 1 502 30 30 G C3' C 67.828 0.3 1 503 30 30 G C8 C 134.13 0.3 1 504 30 30 G N7 N 234.413 0.3 1 505 30 30 G N9 N 167.11 0.3 1 506 31 31 A H1' H 5.753 0.02 1 507 31 31 A H2 H 7.782 0.02 1 508 31 31 A H2' H 4.58 0.02 1 509 31 31 A H8 H 8.082 0.02 1 510 31 31 A C1' C 86.008 0.3 1 511 31 31 A C2 C 149.227 0.3 1 512 31 31 A C2' C 70.309 0.3 1 513 31 31 A C4 C 143.824 0.3 1 514 31 31 A C6 C 153.384 0.3 1 515 31 31 A C8 C 135.743 0.3 1 516 31 31 A N1 N 223.937 0.3 1 517 31 31 A N3 N 214.88 0.3 1 518 31 31 A N7 N 229.872 0.3 1 519 31 31 A N9 N 167.82 0.3 1 520 32 32 A H1' H 5.717 0.02 1 521 32 32 A H2 H 7.997 0.02 1 522 32 32 A H2' H 4.393 0.02 1 523 32 32 A H3' H 4.509 0.02 1 524 32 32 A H8 H 7.978 0.02 1 525 32 32 A C1' C 86.01 0.3 1 526 32 32 A C2 C 149.783 0.3 1 527 32 32 A C2' C 70.471 0.3 1 528 32 32 A C3' C 68.921 0.3 1 529 32 32 A C4 C 143.963 0.3 1 530 32 32 A C6 C 153.886 0.3 1 531 32 32 A C8 C 135.093 0.3 1 532 32 32 A N1 N 224.595 0.3 1 533 32 32 A N3 N 214.78 0.3 1 534 32 32 A N7 N 230.603 0.3 1 535 32 32 A N9 N 168.596 0.3 1 536 33 33 U H1' H 5.557 0.02 1 537 33 33 U H2' H 4.104 0.02 1 538 33 33 U H3' H 4.395 0.02 1 539 33 33 U H5 H 5.373 0.02 1 540 33 33 U H6 H 7.482 0.02 1 541 33 33 U C1' C 86.183 0.3 1 542 33 33 U C2' C 70.168 0.3 1 543 33 33 U C3' C 71.087 0.3 1 544 33 33 U C5 C 99.360 0.3 1 545 33 33 U C6 C 136.897 0.3 1 546 33 33 U N1 N 143.528 0.3 1 547 34 34 U H1' H 5.897 0.02 1 548 34 34 U H2' H 4.334 0.02 1 549 34 34 U H3' H 4.639 0.02 1 550 34 34 U H4' H 4.358 0.02 1 551 34 34 U H5 H 5.726 0.02 1 552 34 34 U H5' H 4.106 0.02 2 553 34 34 U H5'' H 4.031 0.02 2 554 34 34 U H6 H 7.719 0.3 1 555 34 34 U C1' C 85.678 0.3 1 556 34 34 U C2' C 69.937 0.3 1 557 34 34 U C3' C 71.081 0.3 1 558 34 34 U C4' C 79.708 0.3 1 559 34 34 U C5 C 99.726 0.3 1 560 34 34 U C5' C 62.102 0.3 1 561 34 34 U C6 C 138.449 0.3 1 562 34 34 U N1 N 143.287 0.3 1 563 35 35 A H1' H 5.786 0.02 1 564 35 35 A H2 H 8.263 0.02 1 565 35 35 A H2' H 4.755 0.02 1 566 35 35 A H3' H 4.613 0.02 1 567 35 35 A H4' H 4.343 0.02 1 568 35 35 A H8 H 8.252 0.02 1 569 35 35 A H61 H 7.758 0.02 2 570 35 35 A H62 H 7.01 0.02 2 571 35 35 A C1' C 87.528 0.3 1 572 35 35 A C2 C 151.853 0.3 1 573 35 35 A C2' C 70.242 0.3 1 574 35 35 A C3' C 66.53 0.3 1 575 35 35 A C4 C 143.066 0.3 1 576 35 35 A C4' C 76.714 0.3 1 577 35 35 A C6 C 154.723 0.3 1 578 35 35 A C8 C 135.893 0.3 1 579 35 35 A N1 N 228.715 0.3 1 580 35 35 A N3 N 206.807 0.3 1 581 35 35 A N6 N 83.06 0.3 1 582 35 35 A N9 N 168.729 0.3 1 583 36 36 U H1' H 5.32 0.02 1 584 36 36 U H2' H 4.166 0.02 1 585 36 36 U H3 H 10.931 0.02 1 586 36 36 U H3' H 4.253 0.02 1 587 36 36 U H4' H 4.379 0.02 1 588 36 36 U H5 H 5.197 0.02 1 589 36 36 U H6 H 7.439 0.02 1 590 36 36 U C1' C 88.693 0.3 1 591 36 36 U C2' C 70.067 0.3 1 592 36 36 U C3' C 66.434 0.3 1 593 36 36 U C4' C 77.237 0.3 1 594 36 36 U C5 C 97.566 0.3 1 595 36 36 U C6 C 135.005 0.3 1 596 36 36 U N3 N 156.962 0.3 1 597 37 37 U H1' H 6.071 0.02 1 598 37 37 U H2' H 4.152 0.02 1 599 37 37 U H3' H 4.397 0.02 1 600 37 37 U H4' H 4.618 0.02 1 601 37 37 U H5 H 5.664 0.02 1 602 37 37 U H5' H 4.138 0.02 2 603 37 37 U H5'' H 4.034 0.02 2 604 37 37 U H6 H 7.699 0.3 1 605 37 37 U C1' C 84.328 0.3 1 606 37 37 U C2' C 69.996 0.3 1 607 37 37 U C3' C 71.205 0.3 1 608 37 37 U C4' C 80.329 0.3 1 609 37 37 U C5 C 100.725 0.3 1 610 37 37 U C5' C 62.115 0.3 1 611 37 37 U C6 C 137.067 0.3 1 612 37 37 U N1 N 141.517 0.3 1 613 38 38 G H1 H 12.089 0.02 1 614 38 38 G H1' H 5.291 0.02 1 615 38 38 G H2' H 4.54 0.02 1 616 38 38 G H3' H 3.853 0.02 1 617 38 38 G H4' H 4.394 0.02 1 618 38 38 G H5' H 4.084 0.02 2 619 38 38 G H5'' H 3.988 0.02 2 620 38 38 G H8 H 6.811 0.02 1 621 38 38 G H21 H 7.928 0.02 2 622 38 38 G C1' C 88.208 0.3 1 623 38 38 G C2 C 150.322 0.3 1 624 38 38 G C2' C 68.539 0.3 1 625 38 38 G C3' C 69.18 0.3 1 626 38 38 G C4' C 78.152 0.3 1 627 38 38 G C5 C 115.095 0.3 1 628 38 38 G C5' C 63.919 0.3 1 629 38 38 G C6 C 155.062 0.3 1 630 38 38 G C8 C 129.07 0.3 1 631 38 38 G N1 N 147.283 0.3 1 632 38 38 G N2 N 71.329 0.3 1 633 38 38 G N7 N 229.948 0.3 1 634 38 38 G N9 N 166.518 0.3 1 635 39 39 G H1 H 12.408 0.02 1 636 39 39 G H1' H 5.451 0.02 1 637 39 39 G H2' H 4.612 0.02 1 638 39 39 G H3' H 4.534 0.02 1 639 39 39 G H4' H 4.352 0.02 1 640 39 39 G H5' H 4.121 0.02 2 641 39 39 G H5'' H 4.034 0.02 2 642 39 39 G H8 H 6.902 0.02 1 643 39 39 G H21 H 8.228 0.02 2 644 39 39 G C1' C 88.196 0.3 1 645 39 39 G C2 C 150.199 0.3 1 646 39 39 G C2' C 69.625 0.3 1 647 39 39 G C3' C 66.608 0.3 1 648 39 39 G C4' C 76.829 0.3 1 649 39 39 G C5 C 114.618 0.3 1 650 39 39 G C5' C 62.064 0.3 1 651 39 39 G C6 C 154.881 0.3 1 652 39 39 G C8 C 130.334 0.3 1 653 39 39 G N1 N 145.185 0.3 1 654 39 39 G N2 N 72.393 0.3 1 655 39 39 G N7 N 233.042 0.3 1 656 39 39 G N9 N 167.48 0.3 1 657 40 40 A H1' H 5.658 0.02 1 658 40 40 A H2 H 7.443 0.02 1 659 40 40 A H2' H 4.452 0.02 1 660 40 40 A H3' H 4.349 0.02 1 661 40 40 A H8 H 7.839 0.02 1 662 40 40 A H61 H 8.475 0.02 2 663 40 40 A H62 H 5.878 0.02 2 664 40 40 A C1' C 86.854 0.3 1 665 40 40 A C2 C 148.806 0.3 1 666 40 40 A C2' C 70.156 0.3 1 667 40 40 A C3' C 66.9 0.3 1 668 40 40 A C4 C 141.438 0.3 1 669 40 40 A C6 C 153.967 0.3 1 670 40 40 A C8 C 132.768 0.3 1 671 40 40 A N1 N 222.49 0.3 1 672 40 40 A N3 N 207.78 0.3 1 673 40 40 A N6 N 84.014 0.3 1 674 40 40 A N7 N 226.752 0.3 1 675 40 40 A N9 N 169.971 0.3 1 676 41 41 G H1 H 13.733 0.02 1 677 41 41 G H1' H 5.289 0.02 1 678 41 41 G H2' H 4.08 0.02 1 679 41 41 G H3' H 4.215 0.02 1 680 41 41 G H4' H 4.217 0.02 1 681 41 41 G H5' H 4.253 0.02 2 682 41 41 G H5'' H 3.869 0.02 2 683 41 41 G H8 H 6.793 0.02 1 684 41 41 G C1' C 86.868 0.3 1 685 41 41 G C2 C 151.564 0.3 1 686 41 41 G C2' C 69.921 0.3 1 687 41 41 G C3' C 66.829 0.3 1 688 41 41 G C4' C 76.183 0.3 1 689 41 41 G C5 C 114.69 0.3 1 690 41 41 G C5' C 59.56 0.3 1 691 41 41 G C6 C 155.852 0.3 1 692 41 41 G C8 C 128.747 0.3 1 693 41 41 G N1 N 147.439 0.3 1 694 41 41 G N7 N 233.135 0.3 1 695 41 41 G N9 N 168.338 0.3 1 696 42 42 C H1' H 5.17 0.02 1 697 42 42 C H2' H 4.013 0.02 1 698 42 42 C H3' H 4.189 0.02 1 699 42 42 C H4' H 4.11 0.02 1 700 42 42 C H5 H 5.03 0.02 1 701 42 42 C H6 H 7.174 0.02 1 702 42 42 C H41 H 8.113 0.02 2 703 42 42 C H42 H 6.74 0.02 2 704 42 42 C C1' C 88.528 0.3 1 705 42 42 C C2' C 70.092 0.3 1 706 42 42 C C3' C 66.732 0.3 1 707 42 42 C C4' C 76.509 0.3 1 708 42 42 C C5 C 92.146 0.3 1 709 42 42 C C6 C 134.145 0.3 1 710 42 42 C N1 N 149.18 0.3 1 711 42 42 C N3 N 196.413 0.3 1 712 42 42 C N4 N 97.695 0.3 1 713 43 43 A H1' H 6.105 0.02 1 714 43 43 A H2 H 7.45 0.02 1 715 43 43 A H2' H 4.516 0.02 1 716 43 43 A H3' H 4.851 0.02 1 717 43 43 A H4' H 4.299 0.02 1 718 43 43 A H5' H 4.302 0.02 2 719 43 43 A H5'' H 3.942 0.02 2 720 43 43 A H8 H 7.81 0.02 1 721 43 43 A C1' C 85.66 0.3 1 722 43 43 A C2 C 149.153 0.3 1 723 43 43 A C2' C 79.468 0.3 1 724 43 43 A C3' C 72.673 0.3 1 725 43 43 A C4 C 144.356 0.3 1 726 43 43 A C4' C 80.242 0.3 1 727 43 43 A C5' C 60.387 0.3 1 728 43 43 A C6 C 153.905 0.3 1 729 43 43 A C8 C 135.123 0.3 1 730 43 43 A N1 N 224.584 0.3 1 731 43 43 A N3 N 214.956 0.3 1 732 43 43 A N7 N 232.564 0.3 1 733 43 43 A N9 N 166.743 0.3 1 stop_ save_ save_assigned_chem_shift_list_1_2 _Saveframe_category assigned_chemical_shifts _Details . loop_ _Experiment_label '2D 1H-15N HSQC' '2D 1H-15N HSQC NH2 only' '2D 1H-13C HSQC aliphatic' '2D 1H-13C HSQC aromatic' '2D 1H-1H NOESY' '3D 1H-13C NOESY aromatic' '3D 1H-13C NOESY aliphatic' '3D HCCH-TOCSY' '3D HCCH-COSY' '1D 1H-HS11ECHO' '2D 1H-15N HNN-COSY' '2D 1H-13C HNCO' '2D 1H-13C H5C5(C4N)H' '2D 1H-15N HCN aromatic' '2D 1H-15N HCN aliphatic' '2D 1H-15N 2bond-HSQC' 'TROSY relayed HCCH-COSY' '2D 1H-13C long-rangeH8(C8)C5(N1)H1' '2D lr-1H,15N-HSQC' stop_ loop_ _Sample_label $13C15N $13C15N-U $13C15N-AC $13C15N-G $15N $unlab $13C15N-AC_D2O $13C15N-U_D2O $13C15N-G_D2O $13C15N-U_13C15N-SAH $13C15N-SAH stop_ _Sample_conditions_label $298K _Chem_shift_reference_set_label $chemical_shift_reference_1 _Mol_system_component_name SAH _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 76 1 SAH H1' H 5.111 0.02 1 2 76 1 SAH H2 H 7.889 0.02 1 3 76 1 SAH H2' H 3.89 0.02 1 4 76 1 SAH H3' H 2.124 0.02 1 5 76 1 SAH H4' H 2.983 0.02 1 6 76 1 SAH H5' H 2.251 0.02 2 7 76 1 SAH H5'' H 2.335 0.02 2 8 76 1 SAH H8 H 7.397 0.02 1 9 76 1 SAH HA H 3.777 0.02 1 10 76 1 SAH HB1 H 2.13 0.02 4 11 76 1 SAH HB2 H 1.779 0.02 4 12 76 1 SAH HG1 H 2.572 0.02 4 13 76 1 SAH HG2 H 2.275 0.02 4 14 76 1 SAH C1' C 84.04 0.3 1 15 76 1 SAH C2 C 149.511 0.3 1 16 76 1 SAH C2' C 72.776 0.3 1 17 76 1 SAH C3' C 69.243 0.3 1 18 76 1 SAH C4' C 82.649 0.3 1 19 76 1 SAH C5' C 30.718 0.3 1 20 76 1 SAH C8 C 136.526 0.3 1 21 76 1 SAH CA C 51.175 0.3 1 22 76 1 SAH CB C 28.86 0.3 1 23 76 1 SAH CG C 27.118 0.3 1 24 76 1 SAH N7 N 225.71 0.3 1 stop_ save_